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_4321832
_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            'C10 H9 Br3 Cu3 N2 O'
_chemical_formula_weight         603.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.542(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.907(3)
_cell_length_b                   6.0677(13)
_cell_length_c                   21.620(5)
_cell_measurement_temperature    120(2)
_cell_volume                     1430.8(6)
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8190
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    12.785
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.589018
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.00051(10)
_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   0.986
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_obs          0.0370
_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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0786
_refine_ls_wR_factor_obs         0.0718
_reflns_number_observed          2453
_reflns_number_total             3358
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980997v_1.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
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^)+(0.0355P)^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^)+(0.0355P)^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_database_code               4321832