 
data_21
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C40 H42 Ca N4 O8' 
_chemical_formula_sum 
 'C40 H42 Ca N4 O8' 
_chemical_formula_weight          746.85 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ca'  'Ca'   0.2262   0.3064 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       triclinic 
_space_group_IT_number            2 
_space_group_name_H-M_alt         'P -1' 
_space_group_name_Hall            '-P 1' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    8.9649(7) 
_cell_length_b                    9.8594(7) 
_cell_length_c                    10.9919(6) 
_cell_angle_alpha                 91.671(5) 
_cell_angle_beta                  93.659(5) 
_cell_angle_gamma                 101.084(6) 
_cell_volume                      950.65(11) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     1417 
_cell_measurement_theta_min       2.7940 
_cell_measurement_theta_max       27.7860 
  
_exptl_crystal_description        needles 
_exptl_crystal_colour             'Colourless platy' 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.305 
_exptl_crystal_F_000              394 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.305 
_exptl_crystal_size_mid           0.156 
_exptl_crystal_size_min           0.039 
_exptl_absorpt_coefficient_mu     0.222 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.954 
_exptl_absorpt_correction_T_max   0.990 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'Enhance (Mo) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur 3 E' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  16.0382 
_diffrn_reflns_number             5599 
_diffrn_reflns_av_unetI/netI      0.0595 
_diffrn_reflns_av_R_equivalents   0.0232 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.750 
_diffrn_reflns_theta_max          28.277 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.801 
_diffrn_measured_fraction_theta_full  0.988 
_diffrn_reflns_Laue_measured_fraction_max    0.801 
_diffrn_reflns_Laue_measured_fraction_full   0.988 
_diffrn_reflns_point_group_measured_fraction_max   0.801 
_diffrn_reflns_point_group_measured_fraction_full  0.988 
_reflns_number_total              3772 
_reflns_number_gt                 2690 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0492P)²+0.4148P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    mixed 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          3772 
_refine_ls_number_parameters      247 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0770 
_refine_ls_R_factor_gt            0.0493 
_refine_ls_wR_factor_ref          0.1276 
_refine_ls_wR_factor_gt           0.1142 
_refine_ls_goodness_of_fit_ref    1.018 
_refine_ls_restrained_S_all       1.018 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ca1 Ca 1.000000 0.500000 0.500000 0.0300(2) Uani 1 2 d S . P . . 
N1 N 0.4027(2) 0.4029(2) 0.34003(17) 0.0271(5) Uani 1 1 d . . . . . 
N2 N 0.5018(2) 0.3429(2) 0.41247(17) 0.0255(5) Uani 1 1 d . . . . . 
C3 C 0.6505(3) 0.4081(3) 0.4089(2) 0.0252(5) Uani 1 1 d . . . . . 
O3 O 0.75950(18) 0.36943(18) 0.46733(15) 0.0315(4) Uani 1 1 d . . . . . 
C4 C 0.6458(2) 0.5183(2) 0.3264(2) 0.0237(5) Uani 1 1 d . . . . . 
C5 C 0.4895(3) 0.5065(3) 0.2903(2) 0.0276(6) Uani 1 1 d . . . . . 
H5A H 0.451283 0.566893 0.235949 0.033 Uiso 1 1 calc R U . . . 
C6 C 0.4456(3) 0.2141(3) 0.4711(2) 0.0295(6) Uani 1 1 d . . . . . 
H6A H 0.353323 0.223312 0.512931 0.035 Uiso 1 1 calc R U . . . 
H6B H 0.523943 0.198157 0.533807 0.035 Uiso 1 1 calc R U . . . 
C7 C 0.4075(3) 0.0904(3) 0.3827(2) 0.0266(5) Uani 1 1 d . . . . . 
C8 C 0.2758(3) -0.0074(3) 0.3883(2) 0.0303(6) Uani 1 1 d . . . . . 
H8A H 0.206313 0.005429 0.447284 0.036 Uiso 1 1 calc R U . . . 
C9 C 0.2417(3) -0.1247(3) 0.3097(2) 0.0309(6) Uani 1 1 d . . . . . 
H9A H 0.151156 -0.191386 0.316460 0.037 Uiso 1 1 calc R U . . . 
C10 C 0.3401(3) -0.1430(3) 0.2223(2) 0.0301(6) Uani 1 1 d . . . . . 
C11 C 0.4732(3) -0.0462(3) 0.2154(2) 0.0363(6) Uani 1 1 d . . . . . 
H11A H 0.542119 -0.058980 0.155847 0.044 Uiso 1 1 calc R U . . . 
C12 C 0.5062(3) 0.0684(3) 0.2942(2) 0.0341(6) Uani 1 1 d . . . . . 
H12A H 0.597996 0.133744 0.288261 0.041 Uiso 1 1 calc R U . . . 
O13 O 0.3167(2) -0.25287(19) 0.13815(17) 0.0392(5) Uani 1 1 d . . . . . 
C14 C 0.1802(3) -0.3525(3) 0.1417(3) 0.0461(7) Uani 1 1 d . . . . . 
H14A H 0.179681 -0.427784 0.081376 0.069 Uiso 1 1 calc R U . . . 
H14B H 0.092502 -0.308818 0.122838 0.069 Uiso 1 1 calc R U . . . 
H14C H 0.173934 -0.389714 0.223310 0.069 Uiso 1 1 calc R U . . . 
C15 C 0.7741(3) 0.6138(2) 0.2929(2) 0.0255(5) Uani 1 1 d . . . . . 
O15 O 0.90307(18) 0.62695(18) 0.34817(15) 0.0325(4) Uani 1 1 d . . . . . 
C16 C 0.7610(3) 0.7015(3) 0.1855(2) 0.0263(5) Uani 1 1 d . . . . . 
C17 C 0.8462(3) 0.8360(3) 0.1890(2) 0.0317(6) Uani 1 1 d . . . . . 
H17A H 0.905273 0.872868 0.261496 0.038 Uiso 1 1 calc R U . . . 
C18 C 0.8452(3) 0.9159(3) 0.0878(3) 0.0378(6) Uani 1 1 d . . . . . 
H18A H 0.904588 1.006971 0.090838 0.045 Uiso 1 1 calc R U . . . 
C19 C 0.7589(3) 0.8645(3) -0.0171(3) 0.0425(7) Uani 1 1 d . . . . . 
H19A H 0.758071 0.920092 -0.086182 0.051 Uiso 1 1 calc R U . . . 
C20 C 0.6735(3) 0.7320(3) -0.0221(2) 0.0445(7) Uani 1 1 d . . . . . 
H20A H 0.613559 0.696336 -0.094474 0.053 Uiso 1 1 calc R U . . . 
C21 C 0.6752(3) 0.6508(3) 0.0788(2) 0.0354(6) Uani 1 1 d . . . . . 
H21A H 0.616774 0.559365 0.074662 0.043 Uiso 1 1 calc R U . . . 
O30 O 1.09314(18) 0.3593(2) 0.35875(17) 0.0435(5) Uani 1 1 d D . . . . 
H30 H 1.1933(3) 0.3627(18) 0.3522(16) 0.069(11) Uiso 1 1 d D . . . . 
C31 C 1.0062(3) 0.2486(3) 0.2818(3) 0.0478(8) Uani 1 1 d . . . . . 
H31A H 0.929601 0.191300 0.329492 0.057 Uiso 1 1 calc R U . . . 
H31B H 1.074646 0.189112 0.252065 0.057 Uiso 1 1 calc R U . . . 
C32 C 0.9277(4) 0.3025(4) 0.1758(3) 0.0620(10) Uani 1 1 d . . . . . 
H32A H 1.003420 0.345779 0.121107 0.093 Uiso 1 1 calc R U . . . 
H32B H 0.870859 0.371127 0.204786 0.093 Uiso 1 1 calc R U . . . 
H32C H 0.857112 0.225974 0.131708 0.093 Uiso 1 1 calc R U . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ca1 O3 2.2895(16) 2_766 ? 
Ca1 O3 2.2895(16) . ? 
Ca1 O15 2.3370(17) 2_766 ? 
Ca1 O15 2.3370(17) . ? 
Ca1 O30 2.3490(18) 2_766 ? 
Ca1 O30 2.3490(18) . ? 
N1 C5 1.314(3) . ? 
N1 N2 1.383(3) . ? 
N2 C3 1.368(3) . ? 
N2 C6 1.457(3) . ? 
C3 O3 1.261(3) . ? 
C3 C4 1.440(3) . ? 
C4 C5 1.413(3) . ? 
C4 C15 1.416(3) . ? 
C6 C7 1.509(3) . ? 
C7 C8 1.379(3) . ? 
C7 C12 1.395(3) . ? 
C8 C9 1.396(3) . ? 
C9 C10 1.375(3) . ? 
C10 O13 1.379(3) . ? 
C10 C11 1.385(4) . ? 
C11 C12 1.378(4) . ? 
O13 C14 1.418(3) . ? 
C15 O15 1.253(3) . ? 
C15 C16 1.495(3) . ? 
C16 C21 1.386(3) . ? 
C16 C17 1.395(3) . ? 
C17 C18 1.383(4) . ? 
C18 C19 1.374(4) . ? 
C19 C20 1.379(4) . ? 
C20 C21 1.387(4) . ? 
O30 C31 1.432(3) . ? 
C31 C32 1.486(4) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O3 Ca1 O3 180.0 2_766 . ? 
O3 Ca1 O15 80.68(6) 2_766 2_766 ? 
O3 Ca1 O15 99.32(6) . 2_766 ? 
O3 Ca1 O15 99.32(6) 2_766 . ? 
O3 Ca1 O15 80.68(6) . . ? 
O15 Ca1 O15 180.0 2_766 . ? 
O3 Ca1 O30 90.99(6) 2_766 2_766 ? 
O3 Ca1 O30 89.01(6) . 2_766 ? 
O15 Ca1 O30 93.25(7) 2_766 2_766 ? 
O15 Ca1 O30 86.75(7) . 2_766 ? 
O3 Ca1 O30 89.01(6) 2_766 . ? 
O3 Ca1 O30 90.99(6) . . ? 
O15 Ca1 O30 86.75(7) 2_766 . ? 
O15 Ca1 O30 93.25(7) . . ? 
O30 Ca1 O30 180.0 2_766 . ? 
C5 N1 N2 105.16(18) . . ? 
C3 N2 N1 112.79(19) . . ? 
C3 N2 C6 126.8(2) . . ? 
N1 N2 C6 119.97(18) . . ? 
O3 C3 N2 123.2(2) . . ? 
O3 C3 C4 132.1(2) . . ? 
N2 C3 C4 104.71(19) . . ? 
C3 O3 Ca1 124.42(16) . . ? 
C5 C4 C15 130.2(2) . . ? 
C5 C4 C3 104.6(2) . . ? 
C15 C4 C3 125.3(2) . . ? 
N1 C5 C4 112.8(2) . . ? 
N2 C6 C7 113.11(19) . . ? 
C8 C7 C12 117.3(2) . . ? 
C8 C7 C6 121.4(2) . . ? 
C12 C7 C6 121.3(2) . . ? 
C7 C8 C9 121.9(2) . . ? 
C10 C9 C8 119.5(2) . . ? 
C9 C10 O13 124.7(2) . . ? 
C9 C10 C11 119.5(2) . . ? 
O13 C10 C11 115.9(2) . . ? 
C12 C11 C10 120.4(2) . . ? 
C11 C12 C7 121.3(2) . . ? 
C10 O13 C14 117.2(2) . . ? 
O15 C15 C4 122.7(2) . . ? 
O15 C15 C16 117.0(2) . . ? 
C4 C15 C16 120.3(2) . . ? 
C15 O15 Ca1 132.32(16) . . ? 
C21 C16 C17 118.4(2) . . ? 
C21 C16 C15 122.3(2) . . ? 
C17 C16 C15 119.2(2) . . ? 
C18 C17 C16 120.5(2) . . ? 
C19 C18 C17 120.4(3) . . ? 
C18 C19 C20 119.9(3) . . ? 
C19 C20 C21 119.9(3) . . ? 
C16 C21 C20 120.8(3) . . ? 
C31 O30 Ca1 127.10(15) . . ? 
O30 C31 C32 111.1(3) . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag 
O30 H30 N1  0.9000(1) 1.856(4) 2.747(2) 170.0(17) 1_655 yes 
  
_refine_diff_density_max    0.514 
_refine_diff_density_min   -0.423 
_refine_diff_density_rms    0.051 
  
  
  
#===END

