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_7250206
_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         '2(C2 H6 O S), C38 H24 O8'
_chemical_formula_sum            'C42 H36 O10 S2'
_chemical_formula_weight         764.83
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-18 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                105.538(2)
_cell_angle_beta                 95.126(2)
_cell_angle_gamma                101.433(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8684(2)
_cell_length_b                   13.8322(4)
_cell_length_c                   14.4683(5)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.45
_cell_volume                     1283.20(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      292.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_min         1.815
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7383
_exptl_absorpt_correction_T_min  0.6777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.9179.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_platon_squeeze_details          'Spek, A. L. (2015). Acta Cryst. C71, 9-18'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         7485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1404P)^2^+0.3677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5700
_reflns_number_total             7485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00145e2.cif
_cod_data_source_block           hl61_a_sq
_cod_depositor_comments
'Adding full bibliography for 7250204--7250207.cif.'
_cod_original_cell_volume        1283.19(7)
_cod_database_code               7250206
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.957
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C6(H6), C7(H7), C9(H9), C11(H11), C14(H14), C15(H15),
 C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              3465
_shelx_fab_checksum              52683
_olex2_submission_special_instructions 'No special instructions were received'