Structural variety in calcium metal–organic frameworks with a tetratopic carboxylate ligand
Zhao, Baiwen; Clarkson, Guy J.; Liu, Jie; Le, Thi Huong; Marrot, Jérôme; Millange, Franck; Frigoli, Michel; Walton, Richard I.; CrystEngComm 27 (2025) 2830–2840; doi:10.1039/D5CE00145E

data_7250204
_publ_section_title
;
 Structural variety in calcium metal--organic frameworks with a tetratopic
 carboxylate ligand
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2830
_journal_page_last               2840
_journal_paper_doi               10.1039/D5CE00145E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C46 H40 Ca N2 O10'
_chemical_formula_sum            'C46 H40 Ca N2 O10'
_chemical_formula_weight         820.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7181)
;
_audit_update_record
;
2025-03-18 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.910(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6216(6)
_cell_length_b                   35.2831(8)
_cell_length_c                   10.5028(3)
_cell_measurement_reflns_used    7647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      1.91
_cell_volume                     5920.6(3)
_computing_cell_refinement       'XDS package'
_computing_data_collection       'XDS package'
_computing_data_reduction        'XDS package'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.799
_diffrn_measurement_device_type  'PROXIMA 2A - Synchrotron SOLEIL'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_reflns_av_R_equivalents  0.2119
_diffrn_reflns_av_unetI/netI     0.1908
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29282
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         27.667
_diffrn_reflns_theta_min         2.369
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.1034
_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/[\s^2^(Fo^2^)+(0.1439P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.2924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2551
_reflns_number_total             5127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00145e2.cif
_cod_data_source_block           fmf2
_cod_depositor_comments
'Adding full bibliography for 7250204--7250207.cif.'
_cod_database_code               7250204
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.997
_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
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C20(H20)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31463
_shelx_fab_checksum              92284
_olex2_submission_special_instructions 'No special instructions were received'
_olex_squeeze_details
'P. van der Sluis and A. L. Spek, Acta Cryst. (1990). A46, 194-201'