Investigations of the Copper Bromide-2,2'-Dipyridyl System: Hydrothermal Synthesis and Structural Characterization of Molecular Cu3Br4(C10H8N2)2, One-Dimensional CuBr2(C10H8N2), and Two-Dimensional [Cu2(OH)2(C10H8N2)2][Cu4Br6]
Robert P. Hammond; Michael Cavaluzzi; Robert C. Haushalter; Jon A. Zubieta; Inorganic Chemistry 38 (1999) 1288–1292; doi:10.1021/ic980997v

data_4321833
_publ_contact_author
;
     Dr. J. Zubieta
     1-014 Centre for Science and Technology
     Syracuse University
     Syracuse, NY        13244-4100
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_publ_contact_author_email       jazubiet@syr.edu
_publ_contact_author_fax         (315)443-4070
_publ_contact_author_phone       (315)443-2547
_publ_section_title
;
 Investigations of the Copper Bromide-2,2'-Dipyridyl System: Hydrothermal
 Synthesis and Structural Characterization of Molecular Cu3Br4(C10H8N2)2,
 One-Dimensional CuBr2(C10H8N2), and Two-Dimensional
 [Cu2(OH)2(C10H8N2)2][Cu4Br6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1288
_journal_page_last               1292
_journal_paper_doi               10.1021/ic980997v
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source
;
Hydrothermal reaction of copper (I) bromide, copper(II) bromide, and 
(2,2')-dipyridyl
;
_chemical_formula_sum            'C20 H16 Br4 Cu3 N4'
_chemical_formula_weight         822.63
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                61.965(5)
_cell_angle_beta                 68.346(5)
_cell_angle_gamma                69.523(5)
_cell_formula_units_Z            2
_cell_length_a                   10.604(2)
_cell_length_b                   11.642(3)
_cell_length_c                   11.688(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1156.0(5)
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Siemens SMART System'
_diffrn_measurement_method       q-2\q
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7431
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    9.664
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.619520
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.363
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0061(4)
_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   1.051
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    'Not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_obs          0.0408
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0947
_refine_ls_wR_factor_obs         0.0877
_reflns_number_observed          4088
_reflns_number_total             5094
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980997v_2.cif
_cod_data_source_block           (1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' 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 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] 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^)+(0.0396P)^2^+0.0000P] 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        1156.1(4)
_cod_database_code               4321833