Topology-Guided Stepwise Insertion of Three Secondary Linkers in Zirconium Metal-Organic Frameworks.
Zhang, Xin; Frey, Brandon L.; Chen, Yu-Sheng; Zhang, Jian; Journal of the American Chemical Society 140 (2018) 7710–7715; doi:10.1021/jacs.8b04277

data_4132490
_publ_section_title
;
 Topology-Guided Stepwise Insertion of Three Secondary Linkers in
 Zirconium Metal-Organic Frameworks.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7710
_journal_page_last               7715
_journal_paper_doi               10.1021/jacs.8b04277
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C54 H26 O18 Zr3'
_chemical_formula_sum            'C54 H26 O18 Zr3'
_chemical_formula_weight         1236.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.361(3)
_cell_length_b                   33.409(4)
_cell_length_c                   20.691(2)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.91
_cell_measurement_theta_min      2.18
_cell_volume                     16149(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.41325
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31483
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        11.572
_diffrn_reflns_theta_max         11.572
_diffrn_reflns_theta_min         1.178
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.509
_exptl_crystal_description       block
_exptl_crystal_F_000             13420
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1739P)^2^+109.5548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2616
_refine_ls_wR_factor_ref         0.2858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3408
_reflns_number_total             4011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04277_si_010.cif
_cod_data_source_block           NPF-300-6
_cod_database_code               4132490
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C16-C15 = C16-C17 = C18-C17 = C19-C20
 1.38 with sigma of 0.02
 C14-C15 = C18-C19
 1.46 with sigma of 0.02
 O7-C20
 1.35 with sigma of 0.02
 C17-C15 = C16-C18
 2.42 with sigma of 0.04
 C18-C20
 2.48 with sigma of 0.04
3. Rigid bond restraints
 O6, C14, C15, C16, C17, C18, C19, C20, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O6 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim
O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: C20(0.5) O7(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C4(H4), C9(H9), C10(H10), C16(H16), C17(H17)
;
_shelx_res_checksum              64600
_shelx_hkl_checksum              66727
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'