Net-Clipping: An Approach to Deduce the Topology of Metal-Organic Frameworks Built with Zigzag Ligands.
Ortín-Rubio, Borja; Ghasempour, Hosein; Guillerm, Vincent; Morsali, Ali; Juanhuix, Judith; Imaz, Inhar; Maspoch, Daniel; Journal of the American Chemical Society 142 (2020) 9135–9140; doi:10.1021/jacs.0c03404

data_4134914
_publ_section_title
;
 Net-Clipping: An Approach to Deduce the Topology of Metal-Organic
 Frameworks Built with Zigzag Ligands.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9135
_journal_page_last               9140
_journal_paper_doi               10.1021/jacs.0c03404
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '0.06(C168 H96 O72 Tb12)'
_chemical_formula_sum            'C10.5 H6 O4.5 Tb0.75'
_chemical_formula_weight         323.34
_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   geom
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.22(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.290(5)
_cell_length_b                   17.430(5)
_cell_length_c                   24.110(5)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    100
_cell_measurement_theta_max      40
_cell_measurement_theta_min      1
_cell_volume                     7264(3)
_computing_cell_refinement       'xds kabsch, 2010'
_computing_data_collection       'mxcube Gabadinho, 2010'
_computing_data_reduction        'xds kabsch, 2010'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_device_type  'PILATUS DECTRIS 6M'
_diffrn_measurement_method       'w/ scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92168
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         34.035
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    4.360
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         14980
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+12.4757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13778
_reflns_number_total             14980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03404_si_004.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4134913--4134914.cif.'
_cod_original_formula_sum        'C10.50 H6 O4.50 Tb0.75'
_cod_database_code               4134914
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.580
_shelx_estimated_absorpt_t_min   0.409
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C01B, C9, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C015, C01L, C20, C13, C01K, C017
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C014, C01C, C16, C12, C01J, C01F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C12, C01J, C01F, C014, C01C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C9 \\sim C01B \\sim C11: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C01K) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C01L)
\\sim Ueq, Uanis(C015) \\sim Ueq, Uanis(C017) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C01F) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C014) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00U(H00U), C00V(H00V), C010(H010), C011(H011), C013(H013),
 C018(H018), C019(H019), C9(H9), C11(H11), C01I(H01I), C00Z(H00Z), C12(H12),
 C01J(H01J), C01F(H01F), C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C8(H8),
  C13(H13), C20(H20), C01L(H01L), C017(H017)
4.b Fitted hexagon refined as free rotating group:
 C01B(C9,C11,C01I,C016,C00Z), C16(C12,C01J,C01F,C014,C01C), C13(C20,C01L,C015,
 C017,C01K)
;
_shelx_res_checksum              52434
_shelx_hkl_checksum              13366
_shelx_fab_checksum              47944
_olex2_submission_special_instructions 'No special instructions were received'