A post-synthetically reduced borane-functionalised metal-organic framework with oxidation-inhibiting reactivity
Ablott, Timothy Andrew; Telfer, Shane; Richardson, Christopher; CrystEngComm  (2020) –; doi:10.1039/D0CE00930J

data_7240932
_publ_section_title
;
 A post-synthetically reduced borane-functionalised metal-organic
 framework with oxidation-inhibiting reactivity
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00930J
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H36 O16 Zn4'
_chemical_formula_sum            'C48 H36 O16 Zn4'
_chemical_formula_weight         1130.25
_chemical_name_common            WUF-31
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-28 deposited with the CCDC.	2020-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1805(3)
_cell_length_b                   17.1805(3)
_cell_length_c                   17.1173(6)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    292.0
_cell_measurement_theta_max      74.29
_cell_measurement_theta_min      4.46
_cell_volume                     5052.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_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      292.0
_diffrn_detector
'PHOTON III M28 Charge-Integrating Pixel Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'Helios Optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35740
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        63.658
_diffrn_reflns_theta_max         63.658
_diffrn_reflns_theta_min         5.758
_diffrn_source                   'Bruker IuS DIAMOND'
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.743
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 1532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         4359
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1370P)^2^+8.0522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2433
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3763
_reflns_number_total             4359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00930j3.cif
_cod_data_source_block           WUF-31
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7240932
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.822
_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. Restrained distances
 C21-C21_$1
 2.41 with sigma of 0.02
 C20-C20_$1
 2.41 with sigma of 0.02
 C17-C24
 1.5 with sigma of 0.02
 C19-C21
 2.41 with sigma of 0.04
 C22-C20
 2.41 with sigma of 0.04
 O26-C25
 2.3732 with sigma of 0.04
 O26-C17
 2.4353 with sigma of 0.04
 C17-C25
 2.5114 with sigma of 0.04
3. Others
 Fixed Sof: H8(0.5) H17(0.25) C10(0.5) H10(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) O11(0.5) H11(0.5) C24(0.25) H24(0.25) C25(0.25) H25A(0.25)
 H25B(0.25) H25C(0.25) O26(0.25) H26(0.25)
 Fixed Uiso: C10(0.2) C11(0.2) O11(0.2) C24(0.2) C25(0.2) O26(0.2)
 Fixed X: C10(0.54219) C11(0.556509) O11(0.589469) C24(0.895)
 Fixed Y: C10(0.623831) C11(0.69698) O11(0.63792) C24(0.395)
 Fixed Z: C10(1.19683) C11(1.14695) O11(1.2563) C24(0.669001)
4.a Free rotating group:
 C24(C25)
4.b Ternary CH refined with riding coordinates:
 C10(H10), C24(H24)
4.c Me refined with everything fixed:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C)
4.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C6(H6), C5(H5), C16(H16), C17(H17), C20(H20), C21(H21)
4.e Fitted hexagon refined as free rotating group:
 C4(C9,C8,C7,C6,C5)
4.f Tetrahedral OH refined with everything fixed:
 O11(H11), O26(H26)
;
_shelx_res_checksum              53813
_olex2_exptl_crystal_mounting_method 'Mounted in a polymer sleeve'
_olex2_submission_special_instructions 'No special instructions were received'