Redetermination of the crystal structure of the crystal sponge the poly[tetrakis(μ3-2,4,6-tris(pyridin-4-yl)-1,3,5-triazine)-dodecaiodidohexazinc(II) nitrobenzene solvate], C72H48I12N24Zn6⋅10(C6H5NO2)
Eigner, Václav; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 45–49; doi:10.1515/ncrs-2021-0367

data_8104957
_publ_section_title
;
 Redetermination of the crystal structure of the crystal sponge the
 poly[tetrakis(\m3-2,4,6-tris(pyridin-4-yl)-1,3,5-triazine)-dodecaiodidohexazinc(II)
 nitrobenzene solvate], C72H48I12N24Zn6&#x22C5;10(C6H5NO2)
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              45
_journal_page_last               49
_journal_paper_doi               10.1515/ncrs-2021-0367
_journal_volume                  237
_journal_year                    2022
_chemical_compound_source        .
_chemical_formula_moiety         'C72 H48 I12 N24 Zn6, 10(C6 H5 N O2)'
_chemical_formula_sum            'C132 H98 I12 N34 O20 Zn6'
_chemical_formula_weight         4395.60
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.9033(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.97800(15)
_cell_length_b                   15.02541(6)
_cell_length_c                   30.13247(12)
_cell_measurement_reflns_used    130332
_cell_measurement_temperature    95
_cell_measurement_theta_max      74.04
_cell_measurement_theta_min      2.62
_cell_volume                     15495.86(11)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2020) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2020)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2020) 
;
_computing_molecular_graphics    'Diamond 3.0 (Brandenburg, 1999)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      95
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.060
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            268201
_diffrn_reflns_theta_full        72.780
_diffrn_reflns_theta_max         74.265
_diffrn_reflns_theta_min         2.582
_diffrn_standards_decay_%        .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.394
_exptl_absorpt_correction_T_max  0.21
_exptl_absorpt_correction_T_min  0.03
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
 Gaussian Integration (Busing and Levy, 1957) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8416.050
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.076
_refine_diff_density_max         2.99
_refine_diff_density_min         -2.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1857
_refine_ls_number_reflns         31400
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.0026952
_refine_ls_shift/su_mean         0.0000468
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1329
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1329
_reflns_limit_h_max              42
_reflns_limit_h_min              -43
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                30257
_reflns_number_total             31402
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.16
_oxford_diffrn_Wilson_scale      1.79
_oxford_refine_ls_r_factor_ref   0.0515
_oxford_refine_ls_scale          0.7790(10)
_oxford_reflns_number_all        31400
_cod_data_source_file            suppl_j_ncrs-2021-0367_suppl.cif
_cod_data_source_block           FujiMOF.P21c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               8104957
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0515
_oxford_refine_ls_wr_factor_all  0.1329