Bromine-rich Zinc Bromides: Zn6Br12(18-crown-6)2×(Br2)5, Zn4Br8(18-crown-6)2×(Br2)3, and Zn6Br12(18-crown-6)2\τimes (Br2)2.
Hausmann, David; Feldmann, Claus; Inorganic chemistry 55 (2016) 6141–6147; doi:10.1021/acs.inorgchem.6b00663

data_4347827
_publ_section_title
;
 Bromine-rich Zinc Bromides: Zn6Br12(18-crown-6)2\\times (Br2)5,
 Zn4Br8(18-crown-6)2\\times (Br2)3, and Zn6Br12(18-crown-6)2\\times
 (Br2)2.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6141
_journal_page_last               6147
_journal_paper_doi               10.1021/acs.inorgchem.6b00663
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C12 H24 Br7 O6 Zn2'
_chemical_formula_weight         954.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.48(3)
_cell_angle_beta                 101.72(3)
_cell_angle_gamma                99.71(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2271(16)
_cell_length_b                   10.418(2)
_cell_length_c                   15.527(3)
_cell_measurement_reflns_used    10956
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      1.94
_cell_volume                     1261.4(5)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    13.012
_exptl_absorpt_correction_T_max  0.2570
_exptl_absorpt_correction_T_min  0.1143
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.;X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.0180(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                3994
_reflns_number_total             4816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00663_si_003.cif
_cod_data_source_block           '[Zn2Br7(18-crown-6)]'
_cod_original_cell_volume        1261.4(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4347827