In Situ Selective Ligand Transformation from Si−H to Si−OH for Synergistic Assembly of Hydrogen-bonded Metal−Organic Frameworks
Yuan, Baoling; Tang, Yuan; Gou, Gaozhang; Dan, Wenyan; Li, Liangchun; CrystEngComm  (2020) –; doi:10.1039/D0CE00629G

data_7240499
_publ_section_title
;
 In Situ Selective Ligand Transformation from Si&#x2212;H to Si&#x2212;OH
 for Synergistic Assembly of Hydrogen-bonded Metal&#x2212;Organic
 Frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00629G
_journal_year                    2020
_chemical_formula_moiety         'C45 H39 Mn3 N O18 Si2'
_chemical_formula_sum            'C45 H39 Mn3 N O18 Si2'
_chemical_formula_weight         1102.77
_chemical_name_common            Mn-TPCSiOH
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-04 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7672(2)
_cell_length_b                   25.0553(5)
_cell_length_c                   24.4048(5)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.44
_cell_measurement_theta_min      3.66
_cell_volume                     6514.7(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44590
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.512
_diffrn_reflns_theta_min         2.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.493
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         11984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0390P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8591
_reflns_number_total             11865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00629g2.cif
_cod_data_source_block           SiMOF-2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7240499
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.223
_shelx_estimated_absorpt_t_min   0.054
_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, All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B), O11(H11A,H11B), O10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C6(H6), C12(H12), C16(H16), C15(H15), C13(H13),
 C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30), C31(H31),
  C44(H44), C43(H43), C41(H41), C40(H40), C37(H37), C36(H36), C34(H34),
 C33(H33), C1(H1)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O14(H14)
;
_shelx_res_checksum              12094
_shelx_fab_checksum              96618
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'