Hydrogen-Bond-Assisted Symmetry Breaking in a Network of Chiral Metal-Organic Assemblies.
Rizzuto, Felix J.; Pröhm, Patrick; Plajer, Alex J.; Greenfield, Jake L.; Nitschke, Jonathan R.; Journal of the American Chemical Society 141 (2019) 1707–1715; doi:10.1021/jacs.8b12323

data_4128093
_publ_section_title
;
 Hydrogen-Bond-Assisted Symmetry Breaking in a Network of Chiral
 Metal-Organic Assemblies.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1707
_journal_page_last               1715
_journal_paper_doi               10.1021/jacs.8b12323
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'(Zn3 C153 H135 N27 O9), 5.5(S O3 C F3), 0.5(C B11 H12), 0.25(C6 H14 O), 4(C2 H3 N)'
_chemical_formula_sum
'C168.5 H156.5 B5.5 F16.5 N31 O25.75 S5.5 Zn3'
_chemical_formula_weight         3773.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                107.577(2)
_cell_angle_beta                 104.677(2)
_cell_angle_gamma                111.113(2)
_cell_formula_units_Z            2
_cell_length_a                   22.3184(10)
_cell_length_b                   24.7127(10)
_cell_length_c                   25.3074(11)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      50.47
_cell_measurement_theta_min      3.03
_cell_volume                     11337.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            162410
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        50.672
_diffrn_reflns_theta_max         50.672
_diffrn_reflns_theta_min         2.129
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             3889
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2517
_refine_ls_number_reflns         23822
_refine_ls_number_restraints     4142
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1055
_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^)+(0.1761P)^2^+64.8286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2942
_refine_ls_wR_factor_ref         0.3115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19062
_reflns_number_total             23822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12323_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        11337.4(9)
_cod_original_formula_sum
'C168.50 H156.50 B5.50 F16.50 N31 O25.75 S5.50 Zn3'
_cod_database_code               4128093
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.739
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              26676
_shelx_hkl_checksum              81271
_shelx_fab_checksum              30913