Synthesis and Crystal Structures of (C5H7N3Br)3CuBr4 and (C5H8N3)CuBr2: An Isolated Tetrahedral CuBr43- Anion
Shu-Hui Liu; Jhy-Der Chen; Lin-Shu Liou; Ju-Chun Wang; Inorganic Chemistry 40 (2001) 6499–6501; doi:10.1021/ic010529c

data_4320640
_publ_section_title
;
 Synthesis and Crystal Structures of (C5H7N3Br)3CuBr4 and (C5H8N3)CuBr2:
 An Isolated Tetrahedral CuBr43- Anion
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6499
_journal_page_last               6501
_journal_paper_doi               10.1021/ic010529c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15 H21 Br7 Cu N9'
_chemical_formula_weight         950.32
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1793(6)
_cell_length_b                   24.347(2)
_cell_length_c                   13.7606(9)
_cell_measurement_temperature    298(2)
_cell_volume                     2681.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_method       'phi and omega scans'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            10101
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    11.269
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.3420
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.354
_exptl_crystal_description       Column
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00084(14)
_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_all   1.123
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_obs          0.0559
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+19.5966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1281
_refine_ls_wR_factor_obs         0.1179
_reflns_number_observed          3715
_reflns_number_total             4592
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010529c_1.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+19.5966P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+19.5966P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2681.4(3)
_cod_database_code               4320640