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_4128094
_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
'(C153 H135 N27 ZN3 O9), 6(B F4), 0.5(C4 H10 O), 6.5(C2 H3 N), (H2 O)'
_chemical_formula_sum            'C168 H161.5 B6 F24 N33.5 O10.5 Zn3'
_chemical_formula_weight         3534.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 104.784(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.9958(11)
_cell_length_b                   35.3721(14)
_cell_length_c                   22.2126(7)
_cell_measurement_reflns_used    18467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.8900
_cell_measurement_theta_min      0.9957
_cell_volume                     18989.2(13)
_computing_cell_refinement       'XIA2 0.4.0.331-g9691117'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.331-g9691117'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            93770
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        20.181
_diffrn_reflns_theta_max         20.181
_diffrn_reflns_theta_min         0.817
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9730
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction 
using spherical harmonics
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       rod
_exptl_crystal_F_000             7296
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3067
_refine_ls_number_reflns         19935
_refine_ls_number_restraints     7953
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.1130
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3200
_refine_ls_wR_factor_ref         0.3385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13694
_reflns_number_total             19935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12323_si_004.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C168 H161.50 B6 F24 N33.50 O10.50 Zn3'
_cod_database_code               4128094
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.992
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              45868
_shelx_hkl_checksum              69761
_shelx_fab_checksum              26438