Synthesis and characterization of two metallo-hydrogen-bonded organic frameworks with diverse structures and properties
Zhou, Mi; Wang, Yujiang; Yuan, Guoyuan; Ju, Zhanfeng; Yuan, Daqiang; CrystEngComm 25 (2023) 6132–6136; doi:10.1039/D3CE00917C

data_7247569
_publ_section_title
;
 Synthesis and characterization of two metallo-hydrogen-bonded organic
 frameworks with diverse structures and properties
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              6132
_journal_page_last               6136
_journal_paper_doi               10.1039/D3CE00917C
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration r,r
_chemical_formula_sum            'C45 H69 Cu3 N6 O19 P'
_chemical_formula_weight         1219.65
_chemical_name_systematic        MHOF-PO4-1
_space_group_crystal_system      cubic
_space_group_IT_number           210
_space_group_name_Hall           'F 4d 2 3'
_space_group_name_H-M_alt        'F 41 3 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-08-12 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   37.4254(2)
_cell_length_b                   37.4254(2)
_cell_length_c                   37.4254(2)
_cell_measurement_reflns_used    6060
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      71.9090
_cell_measurement_theta_min      3.8860
_cell_volume                     52420.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15912
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.031
_diffrn_reflns_theta_min         3.917
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             20320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: H2O/MeOH'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1206 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4330
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.687
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3485
_reflns_number_total             4330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00917c2.cif
_cod_data_source_block           MHOF-PO4-1
_cod_depositor_comments
'Adding full bibliography for 7247568--7247569.cif.'
_cod_original_cell_volume        52420.3(8)
_cod_database_code               7247569
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              71064
_shelx_fab_checksum              24729