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_4128091
_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
'0.65(Zn3 C150 H129 N27 O9), 0.35(Zn3 C153 H135 N27 O9), 6(C B11 H12), 5.5(C2 H3 N), 2.35(O C4 H10)'
_chemical_formula_sum            'C177.45 H243.1 B66 N32.5 O11.35 Zn3'
_chemical_formula_weight         3922.70
_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                66.64(3)
_cell_angle_beta                 70.61(3)
_cell_angle_gamma                71.93(3)
_cell_formula_units_Z            2
_cell_length_a                   21.025(4)
_cell_length_b                   24.479(5)
_cell_length_c                   25.666(5)
_cell_measurement_reflns_used    75247
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.4198
_cell_measurement_theta_min      0.8499
_cell_volume                     11193(5)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.9.3-gb491019a-release'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.9.3-gb491019a-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.546-gdf2e0b53-dials-1.9 (Winter, G., 2010)
;
_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 0.989
_diffrn_measured_fraction_theta_max 0.988
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            148313
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         0.898
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.449
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3045
_refine_ls_number_reflns         45261
_refine_ls_number_restraints     6487
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0861
_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^)+(0.1988P)^2^+4.3425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2801
_refine_ls_wR_factor_ref         0.2922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34664
_reflns_number_total             45261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12323_si_005.cif
_cod_data_source_block           p1-_a_sq
_cod_original_formula_sum        'C177.45 H243.10 B66 N32.50 O11.35 Zn3'
_cod_database_code               4128091
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.934
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58108
_shelx_hkl_checksum              71835
_shelx_fab_checksum              78073