A mesoporous Zr-based metal-organic framework driven by the assembly of an octatopic linker.
Ortín-Rubio, Borja; Perona-Bermejo, Cristina; Suárez Del Pino, José A; Carmona, Francisco J.; Gándara, Felipe; Navarro, Jorge A. R.; Juanhuix, Judith; Imaz, Inhar; Maspoch, Daniel; Chemical communications (Cambridge, England) 59 (2023) 7803–7806; doi:10.1039/d3cc01831h

data_7131704
_publ_section_title
;
 A mesoporous Zr-based metal-organic framework driven by the assembly of
 an octatopic linker.
;
_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7803
_journal_page_last               7806
_journal_paper_doi               10.1039/d3cc01831h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C87 H44 O36 Zr6, 94[C3H7ON]'
_chemical_formula_sum            'C369 H702 N94 O130 Zr6'
_chemical_formula_weight         9083.52
_space_group_crystal_system      cubic
_space_group_IT_number           202
_space_group_name_Hall           '-F 2 2 3'
_space_group_name_H-M_alt        'F m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-19 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   59.677(2)
_cell_length_b                   59.677(2)
_cell_length_c                   59.677(2)
_cell_measurement_reflns_used    10067
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.798
_cell_measurement_theta_min      0.687
_cell_volume                     212530(12)
_computing_cell_refinement       'XDS (Kabsch W., 2010)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'XDS (Kabsch W., 2010)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean
'Pilatus DECTRIS 6M, 424 x 435mm active area, 6 Mpixels'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MD2M - Maatel'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.1572
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            297552
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.798
_diffrn_reflns_theta_max         24.798
_diffrn_reflns_theta_min         0.687
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       cube
_exptl_crystal_F_000             116496
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.497
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         10067
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.1167
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3015
_refine_ls_wR_factor_ref         0.3217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6423
_reflns_number_total             10067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01831h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7131704.cif.'
_cod_original_cell_volume        212530(21)
_cod_database_code               7131704
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C3_$2-C3
 1.38 with sigma of 0.02
 C3-C7
 1.38 with sigma of 0.02
 C1-O2
 1.4 with sigma of 0.02
 C3-C1
 1.5 with sigma of 0.02
3. Restrained planarity
 C3_$2, C3, C7, C3_$3, C3_$1, C7_$3
 with sigma of 0.1
4. Rigid bond restraints
 C63, C00U, C00R, C00Q, C00S, C00V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C00U \\sim C63 \\sim C00V \\sim C00S \\sim C00Q \\sim C00R: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C63: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C63) \\sim Ueq, Uanis(C00Q) \\sim Ueq, Uanis(C00S) \\sim Ueq, Uanis(C00V)
\\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C00R) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O2) = Uanis(C1)
6. Others
 Fixed Sof: C7(0.25) H7(0.25) C3(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
7.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00I(H00I), C00K(H00K), C00L(H00L), C00N(H00N),
 C00O(H00O), C00P(H00P), C00U(H00U), C00Q(H00Q), C00V(H00V), C7(H7)
7.c Fitted hexagon refined as free rotating group:
 C63(C00U,C00R,C00Q,C00S,C00V)
;
_shelx_res_checksum              27086
_shelx_hkl_checksum              10675
_shelx_fab_checksum              29475
_olex2_submission_special_instructions 'No special instructions were received'