Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs.
Yuan, Shuai; Zhang, Peng; Zhang, Liangliang; Garcia-Esparza, Angel T; Sokaras, Dimosthenis; Qin, Jun-Sheng; Feng, Liang; Day, Gregory S.; Chen, Wenmiao; Drake, Hannah F.; Elumalai, Palani; Madrahimov, Sherzod T.; Sun, Daofeng; Zhou, Hong-Cai; Journal of the American Chemical Society 140 (2018) 10814–10819; doi:10.1021/jacs.8b04886

data_4132569
_publ_section_title
;
 Exposed Equatorial Positions of Metal Centers via Sequential Ligand
 Elimination and Installation in MOFs.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10814
_journal_page_last               10819
_journal_paper_doi               10.1021/jacs.8b04886
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C16 H22 Cl2 Cu N2 O6 S2, 2(C2 H6 O S)'
_chemical_formula_sum            'C20 H34 Cl2 Cu N2 O8 S4'
_chemical_formula_weight         693.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                71.8866(9)
_cell_angle_beta                 83.9415(10)
_cell_angle_gamma                76.9365(10)
_cell_formula_units_Z            1
_cell_length_a                   7.0833(3)
_cell_length_b                   10.3708(5)
_cell_length_c                   10.9549(5)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.747
_cell_measurement_theta_min      4.249
_cell_volume                     744.53(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11845
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         74.744
_diffrn_reflns_theta_min         4.249
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    5.699
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       needle
_exptl_crystal_F_000             359
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0418P)^2^+0.5316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2901
_reflns_number_total             2989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04886_si_002.cif
_cod_data_source_block           CuINA2
_cod_database_code               4132569
_shelx_shelxl_version_number     2014/7
_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.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C11(H11), C20(H20)
2.b Idealised Me refined as rotating group:
 C1AA(H1Aa,H1Ab,H1Ac), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c)
2.c Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              23736
_shelx_hkl_checksum              5565
_olex2_submission_special_instructions 'No special instructions were received'