#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:14:12 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/62/7716271.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716271
loop_
_publ_author_name
'Bhattacharjee, Sudip'
'Chakraborty, Tonmoy'
'Banerjee, Soumadip'
'Das, Abhijit K.'
'Bhaumik, Asim'
_publ_section_title
;
 Construction of a series of pH stable Ca-based MOFs, their CO₂
 adsorption and catalytic activity.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11120
_journal_page_last               11132
_journal_paper_doi               10.1039/d4dt01150c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13.05 H15.05 Ca2 N O12'
_chemical_formula_sum            'C13.05 H15.05 Ca2 N O12'
_chemical_formula_weight         458.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                96.156(8)
_cell_angle_beta                 98.994(7)
_cell_angle_gamma                113.548(7)
_cell_formula_units_Z            2
_cell_length_a                   9.2135(19)
_cell_length_b                   10.112(2)
_cell_length_c                   10.455(2)
_cell_measurement_reflns_used    5925
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      25.695
_cell_measurement_theta_min      2.236
_cell_volume                     866.3(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      166.52
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7790
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.237
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1379 before and 0.0701 after correction.
The Ratio of minimum to maximum transmission is 0.6682.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             473
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.581
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2971
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0419P)²+1.2637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2757
_reflns_number_total             2971
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01150c2.cif
_cod_data_source_block           mo_ab170223_0m_a
_cod_depositor_comments
'Adding full bibliography for 7716268--7716271.cif.'
_cod_database_code               7716271
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ca2-H10A \\sim Ca2-H10B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11B) = Uanis(C11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C12B) = Uanis(C12A)
4. Others
 Fixed Sof: C11A(0.7) H11C(0.7) C12A(0.75) H12A(0.75) H12B(0.75) H12C(0.75)
 C13A(0.75) H13A(0.75) H13B(0.75) H13C(0.75) C11B(0.35) H11D(0.35) C12B(0.25)
 H12D(0.25) H12E(0.25) H12F(0.25) C13B(0.25) H13D(0.25) H13E(0.25) H13F(0.25)
5.a Free rotating group:
 O10(H10A,H10B)
5.b Rotating group:
 O9(H9A,H9B), O11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C11A(H11C), C11B(H11D)
5.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C12B(H12D,H12E,H12F), C13B(H13D,
 H13E,H13F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ca2 Ca 0.76747(5) 0.37946(5) 0.46801(4) 0.00729(18) Uani 1 1 d D . . . .
Ca1 Ca 0.47551(6) 0.04898(5) 0.18017(4) 0.00908(19) Uani 1 1 d . . . . .
O8 O 1.26755(19) 0.38844(18) 0.52847(17) 0.0133(4) Uani 1 1 d . . . . .
O4 O 0.5649(2) 0.30377(17) 0.26257(16) 0.0121(4) Uani 1 1 d . . . . .
O2 O 0.4307(2) 0.83805(18) 0.00329(16) 0.0121(4) Uani 1 1 d . . . . .
O6 O 0.6864(2) 0.12217(17) 0.40870(17) 0.0127(4) Uani 1 1 d . . . . .
O7 O 1.01876(19) 0.36680(17) 0.45855(16) 0.0102(4) Uani 1 1 d . . . . .
O3 O 0.8076(2) 0.4574(2) 0.24199(17) 0.0174(4) Uani 1 1 d . . . . .
O1 O 0.4347(3) 0.7860(2) 0.20299(17) 0.0209(4) Uani 1 1 d . . . . .
O5 O 0.7528(2) 0.0679(2) 0.22126(17) 0.0193(4) Uani 1 1 d . . . . .
O9 O 0.5240(2) 0.3006(2) 0.55160(18) 0.0192(4) Uani 1 1 d . . . . .
H9A H 0.547910 0.302459 0.636198 0.029 Uiso 1 1 d R U . . .
H9B H 0.482912 0.364593 0.545461 0.029 Uiso 1 1 d R U . . .
O10 O 0.8575(2) 0.3665(2) 0.69259(19) 0.0273(5) Uani 1 1 d G . . . .
H10A H 0.955899 0.412788 0.739881 0.041 Uiso 1 1 d DG U . . .
H10B H 0.799258 0.327929 0.748209 0.041 Uiso 1 1 d DG U . . .
O11 O 0.3242(3) 0.0072(3) 0.3513(2) 0.0360(6) Uani 1 1 d . . . . .
H11A H 0.227053 -0.066493 0.320310 0.054 Uiso 1 1 d R U . . .
H11B H 0.369649 -0.024574 0.414746 0.054 Uiso 1 1 d R U . . .
O12 O 0.2431(2) 0.0662(2) 0.0794(2) 0.0336(5) Uani 1 1 d . . . . .
C1 C 0.4425(3) 0.7571(2) 0.0843(2) 0.0104(5) Uani 1 1 d . . . . .
C10 C 1.1167(3) 0.3115(2) 0.4952(2) 0.0089(5) Uani 1 1 d . . . . .
C5 C 0.6570(3) 0.3973(2) 0.2047(2) 0.0100(5) Uani 1 1 d . . . . .
C8 C 1.0512(3) 0.1506(2) 0.4978(2) 0.0092(5) Uani 1 1 d . . . . .
C7 C 0.9012(3) 0.0488(3) 0.4220(2) 0.0090(5) Uani 1 1 d . . . . .
C4 C 0.5752(3) 0.4457(2) 0.0941(2) 0.0094(5) Uani 1 1 d . . . . .
C2 C 0.4687(3) 0.6224(2) 0.0387(2) 0.0097(5) Uani 1 1 d . . . . .
C3 C 0.5430(3) 0.5661(2) 0.1304(2) 0.0102(5) Uani 1 1 d . . . . .
H3 H 0.572612 0.611223 0.220764 0.012 Uiso 1 1 calc R U . . .
C6 C 0.7754(3) 0.0862(2) 0.3434(2) 0.0104(5) Uani 1 1 d . . . . .
C9 C 1.1464(3) 0.0994(3) 0.5761(2) 0.0095(5) Uani 1 1 d . . . . .
H9 H 1.247420 0.168310 0.629996 0.011 Uiso 1 1 calc R U . . .
N1 N 0.1203(3) 0.2165(3) 0.0409(3) 0.0275(6) Uani 1 1 d . . . . .
C11A C 0.1736(5) 0.1168(4) 0.0060(4) 0.0216(7) Uani 0.7 1 d . . P A -1
H11C H 0.155093 0.081997 -0.085823 0.026 Uiso 0.7 1 calc R U P A -1
C12A C 0.1496(6) 0.2754(5) 0.1836(5) 0.0394(10) Uani 0.75 1 d . . P A -1
H12A H 0.045423 0.251461 0.209226 0.059 Uiso 0.75 1 calc R U P A -1
H12B H 0.212017 0.382316 0.200592 0.059 Uiso 0.75 1 calc R U P A -1
H12C H 0.210659 0.231436 0.234992 0.059 Uiso 0.75 1 calc R U P A -1
C13A C 0.0328(6) 0.2665(5) -0.0505(5) 0.0441(12) Uani 0.75 1 d . . P A -1
H13A H 0.018871 0.215932 -0.140009 0.066 Uiso 0.75 1 calc R U P A -1
H13B H 0.092936 0.372557 -0.044124 0.066 Uiso 0.75 1 calc R U P A -1
H13C H -0.073847 0.245452 -0.030689 0.066 Uiso 0.75 1 calc R U P A -1
C11B C 0.1883(9) 0.1639(9) 0.1131(8) 0.0216(7) Uani 0.35 1 d . . P A -2
H11D H 0.204353 0.196696 0.204945 0.026 Uiso 0.35 1 calc R U P A -2
C12B C 0.0325(18) 0.3093(15) 0.0746(14) 0.0394(10) Uani 0.25 1 d . . P A -2
H12D H -0.084871 0.250037 0.046088 0.059 Uiso 0.25 1 calc R U P A -2
H12E H 0.064677 0.393303 0.029489 0.059 Uiso 0.25 1 calc R U P A -2
H12F H 0.060716 0.344746 0.170106 0.059 Uiso 0.25 1 calc R U P A -2
C13B C 0.0808(18) 0.1720(16) -0.1134(16) 0.0441(12) Uani 0.25 1 d . . P A -2
H13D H 0.104101 0.260231 -0.152442 0.066 Uiso 0.25 1 calc R U P A -2
H13E H -0.034160 0.104666 -0.144824 0.066 Uiso 0.25 1 calc R U P A -2
H13F H 0.147762 0.123487 -0.139210 0.066 Uiso 0.25 1 calc R U P A -2
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'
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
Ca2 Ca2 Ca1 130.69(2) 2_766 . ?
O8 Ca2 Ca2 87.10(4) 2_766 2_766 ?
O8 Ca2 Ca1 116.32(4) 2_766 . ?
O8 Ca2 O3 73.26(6) 2_766 . ?
O8 Ca2 C10 26.40(6) 2_766 2_766 ?
O4 Ca2 Ca2 128.64(5) . 2_766 ?
O4 Ca2 Ca1 34.48(4) . . ?
O4 Ca2 O8 82.19(6) . 2_766 ?
O4 Ca2 O7 122.46(6) . 2_766 ?
O4 Ca2 O3 52.02(6) . . ?
O4 Ca2 C10 101.14(6) . 2_766 ?
O6 Ca2 Ca2 115.11(4) . 2_766 ?
O6 Ca2 Ca1 40.92(4) . . ?
O6 Ca2 O8 155.22(6) . 2_766 ?
O6 Ca2 O4 75.36(6) . . ?
O6 Ca2 O7 150.87(6) . 2_766 ?
O6 Ca2 O7 77.69(6) . . ?
O6 Ca2 O3 100.11(6) . . ?
O6 Ca2 O9 82.83(6) . . ?
O6 Ca2 O10 89.11(7) . . ?
O6 Ca2 C10 171.53(6) . 2_766 ?
O7 Ca2 Ca2 37.54(4) . 2_766 ?
O7 Ca2 Ca2 35.99(4) 2_766 2_766 ?
O7 Ca2 Ca1 149.83(4) 2_766 . ?
O7 Ca2 Ca1 99.64(4) . . ?
O7 Ca2 O8 52.83(5) 2_766 2_766 ?
O7 Ca2 O8 122.94(6) . 2_766 ?
O7 Ca2 O4 117.55(6) . . ?
O7 Ca2 O7 73.53(6) . 2_766 ?
O7 Ca2 O3 79.22(6) 2_766 . ?
O7 Ca2 O3 79.65(6) . . ?
O7 Ca2 O9 148.85(6) . . ?
O7 Ca2 O10 79.32(6) . . ?
O7 Ca2 C10 26.67(6) 2_766 2_766 ?
O7 Ca2 C10 97.57(6) . 2_766 ?
O3 Ca2 Ca2 76.76(4) . 2_766 ?
O3 Ca2 Ca1 70.62(4) . . ?
O3 Ca2 C10 71.96(6) . 2_766 ?
O9 Ca2 Ca2 148.19(5) . 2_766 ?
O9 Ca2 Ca1 80.37(5) . . ?
O9 Ca2 O8 83.04(6) . 2_766 ?
O9 Ca2 O4 79.86(6) . . ?
O9 Ca2 O7 120.80(6) . 2_766 ?
O9 Ca2 O3 128.06(6) . . ?
O9 Ca2 C10 104.31(7) . 2_766 ?
O10 Ca2 Ca2 77.91(5) . 2_766 ?
O10 Ca2 Ca1 127.09(6) . . ?
O10 Ca2 O8 107.12(7) . 2_766 ?
O10 Ca2 O4 152.96(6) . . ?
O10 Ca2 O7 81.33(6) . 2_766 ?
O10 Ca2 O3 154.62(6) . . ?
O10 Ca2 O9 76.29(7) . . ?
O10 Ca2 C10 96.96(7) . 2_766 ?
C10 Ca2 Ca2 60.85(5) 2_766 2_766 ?
C10 Ca2 Ca1 134.86(5) 2_766 . ?
Ca1 Ca1 Ca2 129.75(2) 2_655 . ?
O4 Ca1 Ca2 35.41(4) . . ?
O4 Ca1 Ca1 115.35(4) . 2_655 ?
O4 Ca1 O2 152.08(6) . 1_545 ?
O4 Ca1 O2 77.12(6) . 2_665 ?
O4 Ca1 O6 71.33(5) . . ?
O4 Ca1 O1 153.65(6) . 1_545 ?
O4 Ca1 O5 92.58(6) . . ?
O4 Ca1 O11 86.18(8) . . ?
O4 Ca1 C1 167.33(7) . 1_545 ?
O2 Ca1 Ca2 97.73(4) 2_665 . ?
O2 Ca1 Ca2 150.23(4) 1_545 . ?
O2 Ca1 Ca1 38.23(4) 2_665 2_655 ?
O2 Ca1 Ca1 36.73(4) 1_545 2_655 ?
O2 Ca1 O2 74.96(6) 2_665 1_545 ?
O2 Ca1 O6 122.67(5) 1_545 . ?
O2 Ca1 O6 118.45(6) 2_665 . ?
O2 Ca1 O1 123.39(6) 2_665 1_545 ?
O2 Ca1 O1 51.28(6) 1_545 1_545 ?
O2 Ca1 O5 79.71(6) 2_665 . ?
O2 Ca1 C1 25.80(6) 1_545 1_545 ?
O2 Ca1 C1 98.11(6) 2_665 1_545 ?
O6 Ca1 Ca2 35.96(4) . . ?
O6 Ca1 Ca1 129.86(4) . 2_655 ?
O6 Ca1 C1 101.53(6) . 1_545 ?
O1 Ca1 Ca2 119.26(5) 1_545 . ?
O1 Ca1 Ca1 86.56(4) 1_545 2_655 ?
O1 Ca1 O6 83.48(6) 1_545 . ?
O1 Ca1 C1 25.91(6) 1_545 1_545 ?
O5 Ca1 Ca2 68.20(5) . . ?
O5 Ca1 Ca1 78.51(5) . 2_655 ?
O5 Ca1 O2 82.05(6) . 1_545 ?
O5 Ca1 O6 51.36(6) . . ?
O5 Ca1 O1 76.97(6) . 1_545 ?
O5 Ca1 C1 74.94(7) . 1_545 ?
O11 Ca1 Ca2 78.25(7) . . ?
O11 Ca1 Ca1 151.94(7) . 2_655 ?
O11 Ca1 O2 120.20(8) . 1_545 ?
O11 Ca1 O2 154.76(7) . 2_665 ?
O11 Ca1 O6 72.38(7) . . ?
O11 Ca1 O1 78.77(7) . 1_545 ?
O11 Ca1 O5 120.32(7) . . ?
O11 Ca1 C1 101.86(8) . 1_545 ?
O12 Ca1 Ca2 115.31(6) . . ?
O12 Ca1 Ca1 85.43(6) . 2_655 ?
O12 Ca1 O4 83.51(7) . . ?
O12 Ca1 O2 92.23(7) . 1_545 ?
O12 Ca1 O2 80.27(7) . 2_665 ?
O12 Ca1 O6 142.76(7) . . ?
O12 Ca1 O1 114.20(7) . 1_545 ?
O12 Ca1 O5 159.97(8) . . ?
O12 Ca1 O11 79.13(8) . . ?
O12 Ca1 C1 107.47(7) . 1_545 ?
C1 Ca1 Ca2 136.23(5) 1_545 . ?
C1 Ca1 Ca1 60.69(5) 1_545 2_655 ?
C10 O8 Ca2 91.96(13) . 2_766 ?
Ca1 O4 Ca2 110.11(6) . . ?
C5 O4 Ca2 94.29(13) . . ?
C5 O4 Ca1 119.06(14) . . ?
Ca1 O2 Ca1 105.04(6) 2_665 1_565 ?
C1 O2 Ca1 93.80(14) . 1_565 ?
C1 O2 Ca1 147.37(16) . 2_665 ?
Ca2 O6 Ca1 103.11(6) . . ?
C6 O6 Ca2 115.03(14) . . ?
C6 O6 Ca1 86.31(13) . . ?
Ca2 O7 Ca2 106.47(6) . 2_766 ?
C10 O7 Ca2 147.65(15) . . ?
C10 O7 Ca2 92.45(14) . 2_766 ?
C5 O3 Ca2 87.24(14) . . ?
C1 O1 Ca1 91.17(13) . 1_565 ?
C6 O5 Ca1 96.66(15) . . ?
Ca2 O9 H9A 109.6 . . ?
Ca2 O9 H9B 109.5 . . ?
H9A O9 H9B 104.3 . . ?
Ca2 O10 H10A 126.3 . . ?
Ca2 O10 H10B 128.5 . . ?
H10A O10 H10B 104.5 . . ?
Ca1 O11 H11A 109.9 . . ?
Ca1 O11 H11B 110.6 . . ?
H11A O11 H11B 103.6 . . ?
C11A O12 Ca1 151.9(2) . . ?
C11B O12 Ca1 128.6(4) . . ?
O2 C1 Ca1 60.40(12) . 1_565 ?
O2 C1 O1 121.7(2) . . ?
O2 C1 C2 119.2(2) . . ?
O1 C1 Ca1 62.92(12) . 1_565 ?
O1 C1 C2 119.1(2) . . ?
C2 C1 Ca1 166.34(16) . 1_565 ?
O8 C10 Ca2 61.63(12) . 2_766 ?
O8 C10 O7 121.6(2) . . ?
O8 C10 C8 119.2(2) . . ?
O7 C10 Ca2 60.87(12) . 2_766 ?
O7 C10 C8 119.2(2) . . ?
C8 C10 Ca2 170.78(15) . 2_766 ?
O4 C5 C4 116.9(2) . . ?
O3 C5 O4 123.1(2) . . ?
O3 C5 C4 119.7(2) . . ?
C7 C8 C10 123.0(2) . . ?
C9 C8 C10 118.6(2) . . ?
C9 C8 C7 118.3(2) . . ?
C8 C7 C6 125.3(2) . . ?
C9 C7 C8 119.5(2) 2_756 . ?
C9 C7 C6 115.1(2) 2_756 . ?
C2 C4 C5 124.3(2) 2_665 . ?
C3 C4 C5 116.1(2) . . ?
C3 C4 C2 119.5(2) . 2_665 ?
C4 C2 C1 122.2(2) 2_665 . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 C4 118.3(2) . 2_665 ?
C4 C3 H3 118.9 . . ?
C2 C3 C4 122.2(2) . . ?
C2 C3 H3 118.9 . . ?
O6 C6 C7 115.9(2) . . ?
O5 C6 O6 123.5(2) . . ?
O5 C6 C7 120.2(2) . . ?
C8 C9 H9 118.9 . . ?
C7 C9 C8 122.2(2) 2_756 . ?
C7 C9 H9 118.9 2_756 . ?
C11A N1 C12A 118.3(3) . . ?
C11A N1 C13A 123.4(4) . . ?
C13A N1 C12A 118.3(3) . . ?
C11B N1 C12B 128.9(7) . . ?
C11B N1 C13B 122.8(7) . . ?
C12B N1 C13B 107.4(8) . . ?
O12 C11A N1 126.4(4) . . ?
O12 C11A H11C 116.8 . . ?
N1 C11A H11C 116.8 . . ?
N1 C12A H12A 109.5 . . ?
N1 C12A H12B 109.5 . . ?
N1 C12A H12C 109.5 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N1 C13A H13A 109.5 . . ?
N1 C13A H13B 109.5 . . ?
N1 C13A H13C 109.5 . . ?
H13A C13A H13B 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
O12 C11B H11D 116.2 . . ?
N1 C11B O12 127.5(7) . . ?
N1 C11B H11D 116.2 . . ?
N1 C12B H12D 109.5 . . ?
N1 C12B H12E 109.5 . . ?
N1 C12B H12F 109.5 . . ?
H12D C12B H12E 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
N1 C13B H13D 109.5 . . ?
N1 C13B H13E 109.5 . . ?
N1 C13B H13F 109.5 . . ?
H13D C13B H13E 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
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
Ca2 Ca2 3.8933(12) 2_766 ?
Ca2 Ca1 3.9484(10) . ?
Ca2 O8 2.4907(17) 2_766 ?
Ca2 O4 2.4365(17) . ?
Ca2 O6 2.3807(17) . ?
Ca2 O7 2.3859(17) . ?
Ca2 O7 2.4736(17) 2_766 ?
Ca2 O3 2.6041(19) . ?
Ca2 O9 2.4011(18) . ?
Ca2 O10 2.4004(19) . ?
Ca2 C10 2.829(2) 2_766 ?
Ca1 Ca1 3.9328(12) 2_655 ?
Ca1 O4 2.3803(17) . ?
Ca1 O2 2.4353(17) 2_665 ?
Ca1 O2 2.5201(17) 1_545 ?
Ca1 O6 2.6557(18) . ?
Ca1 O1 2.5753(18) 1_545 ?
Ca1 O5 2.4488(19) . ?
Ca1 O11 2.407(2) . ?
Ca1 O12 2.314(2) . ?
Ca1 C1 2.892(2) 1_545 ?
O8 C10 1.259(3) . ?
O4 C5 1.274(3) . ?
O2 C1 1.261(3) . ?
O6 C6 1.277(3) . ?
O7 C10 1.271(3) . ?
O3 C5 1.247(3) . ?
O1 C1 1.264(3) . ?
O5 C6 1.243(3) . ?
O9 H9A 0.8737 . ?
O9 H9B 0.8736 . ?
O10 H10A 0.8700 . ?
O10 H10B 0.8700 . ?
O11 H11A 0.8863 . ?
O11 H11B 0.8866 . ?
O12 C11A 1.206(4) . ?
O12 C11B 1.318(8) . ?
C1 C2 1.516(3) . ?
C10 C8 1.497(3) . ?
C5 C4 1.513(3) . ?
C8 C7 1.394(3) . ?
C8 C9 1.392(3) . ?
C7 C6 1.510(3) . ?
C7 C9 1.387(3) 2_756 ?
C4 C2 1.401(3) 2_665 ?
C4 C3 1.393(3) . ?
C2 C3 1.391(3) . ?
C3 H3 0.9500 . ?
C9 H9 0.9500 . ?
N1 C11A 1.328(5) . ?
N1 C12A 1.486(5) . ?
N1 C13A 1.417(5) . ?
N1 C11B 1.204(8) . ?
N1 C12B 1.511(13) . ?
N1 C13B 1.571(17) . ?
C11A H11C 0.9500 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C11B H11D 0.9500 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca2 O8 C10 O7 10.9(2) 2_766 . . . ?
Ca2 O8 C10 C8 -169.52(18) 2_766 . . . ?
Ca2 O4 C5 O3 19.8(2) . . . . ?
Ca2 O4 C5 C4 -154.30(17) . . . . ?
Ca2 O6 C6 O5 -88.1(2) . . . . ?
Ca2 O6 C6 C7 98.82(19) . . . . ?
Ca2 O7 C10 Ca2 -126.7(3) . . . 2_766 ?
Ca2 O7 C10 O8 -11.0(2) 2_766 . . . ?
Ca2 O7 C10 O8 -137.7(2) . . . . ?
Ca2 O7 C10 C8 42.7(4) . . . . ?
Ca2 O7 C10 C8 169.44(18) 2_766 . . . ?
Ca2 O3 C5 O4 -18.5(2) . . . . ?
Ca2 O3 C5 C4 155.50(19) . . . . ?
Ca1 O4 C5 O3 -96.0(2) . . . . ?
Ca1 O4 C5 C4 89.8(2) . . . . ?
Ca1 O2 C1 Ca1 125.9(3) 2_665 . . 1_565 ?
Ca1 O2 C1 O1 15.0(2) 1_565 . . . ?
Ca1 O2 C1 O1 140.8(2) 2_665 . . . ?
Ca1 O2 C1 C2 -164.31(18) 1_565 . . . ?
Ca1 O2 C1 C2 -38.4(4) 2_665 . . . ?
Ca1 O6 C6 O5 14.6(2) . . . . ?
Ca1 O6 C6 C7 -158.42(18) . . . . ?
Ca1 O1 C1 O2 -14.6(2) 1_565 . . . ?
Ca1 O1 C1 C2 164.67(19) 1_565 . . . ?
Ca1 O5 C6 O6 -16.0(2) . . . . ?
Ca1 O5 C6 C7 156.79(18) . . . . ?
Ca1 O12 C11A N1 -103.8(6) . . . . ?
Ca1 O12 C11B N1 143.5(6) . . . . ?
Ca1 C1 C2 C4 -107.6(7) 1_565 . . 2_665 ?
Ca1 C1 C2 C3 70.5(7) 1_565 . . . ?
O8 C10 C8 C7 -156.5(2) . . . . ?
O8 C10 C8 C9 21.3(3) . . . . ?
O4 C5 C4 C2 -90.8(3) . . . 2_665 ?
O4 C5 C4 C3 89.1(3) . . . . ?
O2 C1 C2 C4 -23.0(3) . . . 2_665 ?
O2 C1 C2 C3 155.1(2) . . . . ?
O7 C10 C8 C7 23.0(3) . . . . ?
O7 C10 C8 C9 -159.1(2) . . . . ?
O3 C5 C4 C2 94.9(3) . . . 2_665 ?
O3 C5 C4 C3 -85.3(3) . . . . ?
O1 C1 C2 C4 157.7(2) . . . 2_665 ?
O1 C1 C2 C3 -24.2(3) . . . . ?
C1 C2 C3 C4 -177.9(2) . . . . ?
C10 C8 C7 C6 -9.1(4) . . . . ?
C10 C8 C7 C9 176.1(2) . . . 2_756 ?
C10 C8 C9 C7 -176.1(2) . . . 2_756 ?
C5 C4 C3 C2 179.8(2) . . . . ?
C8 C7 C6 O6 -80.6(3) . . . . ?
C8 C7 C6 O5 106.2(3) . . . . ?
C7 C8 C9 C7 1.8(4) . . . 2_756 ?
C4 C2 C3 C4 0.4(4) 2_665 . . . ?
C2 C4 C3 C2 -0.4(4) 2_665 . . . ?
C9 C8 C7 C6 173.0(2) . . . . ?
C9 C8 C7 C9 -1.8(4) . . . 2_756 ?
C9 C7 C6 O6 94.5(2) 2_756 . . . ?
C9 C7 C6 O5 -78.8(3) 2_756 . . . ?
C12A N1 C11A O12 1.0(6) . . . . ?
C13A N1 C11A O12 -177.0(4) . . . . ?
C12B N1 C11B O12 169.1(8) . . . . ?
C13B N1 C11B O12 1.4(12) . . . . ?
