An ionic Fe-based metal–organic-framework with 4′-pyridyl-2,2′:6′,2′′-terpyridine for catalytic hydroboration of alkynes
Zhang, Guoqi; Zheng, Shengping; Neary, Michelle C.; RSC Advances 13 (2023) 2225–2232; doi:10.1039/D2RA08040K

data_7246124
_publ_section_title
;
 An ionic Fe-based metal--organic-framework with
 4&#x2032;-pyridyl-2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridine for
 catalytic hydroboration of alkynes
;
_journal_issue                   4
_journal_name_full               'RSC Advances'
_journal_page_first              2225
_journal_page_last               2232
_journal_paper_doi               10.1039/D2RA08040K
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety
'C80 H56 Cl2 Fe3 N16, 2(Cl6 Fe2 O), 6(C H4 O), 6(H2 O)'
_chemical_formula_sum            'C86 H92 Cl14 Fe7 N16 O14'
_chemical_formula_weight         2461.00
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-01-04 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.840(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.759(2)
_cell_length_b                   44.011(6)
_cell_length_c                   17.302(3)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.30
_cell_volume                     11357(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            201893
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.327
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.140
_platon_squeeze_details
; 
The unit cell contains an additional amount of unknown solvent
that has been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON. 
See: (a) A.L.Spek (2005) PLATON, A Multipurpose Crystallographic 
Tool, Utrecht University, Utrecht, The Netherlands. 
(b) A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13. 
;
_refine_diff_density_max         1.880
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         20069
_refine_ls_number_restraints     2705
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.1335
_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^)+(0.0352P)^2^+483.4871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16166
_reflns_number_total             20069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra08040k2.cif
_cod_data_source_block           gz1135rev_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7246124
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.555
_shelx_estimated_absorpt_t_max   0.843
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              55835
_shelx_fab_checksum              8746