#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:43:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179303 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/00/4320086.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320086
loop_
_publ_author_name
'Roger D. Willett'
'George Pon'
'Callie Nagy'
_publ_section_title
;
 Crystal Chemistry of the 4,4'-Dimethyl-2,2'bipyridine/Copper Bromide
 System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4342
_journal_page_last               4352
_journal_paper_doi               10.1021/ic010229v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H35.06 Br1.94 Cu N4 O5.56'
_chemical_formula_weight         687.15
_chemical_name_systematic
;
  [bis(4,4'-dimethyl-2,2'-bipyridine)copper(II)bromide] bromide/hydroxide
  hydrate

;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.390(3)
_cell_length_b                   7.4869(15)
_cell_length_c                   14.449(3)
_cell_measurement_reflns_used    5476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      1.58
_cell_volume                     1393.4(5)
_computing_cell_refinement       'Siemens SCANS'
_computing_data_collection       'Siemens SCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'ω scan'
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5746
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  'beginning and end'
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    3.608
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pleochroic green/brown'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin slats'
_exptl_crystal_F_000             697
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          <0.02?
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0022(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         1968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0647P)²+2.8695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                1644
_reflns_number_total             1968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010229v_3.cif
_cod_data_source_block           Compound2'-233p2c
_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 
;
_cod_original_cell_volume        1393.5(5)
_cod_database_code               4320086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.60293(15) 1.2500 0.0500(4) Uani 1 2 d S . .
Br1 Br 0.5000 0.26701(13) 1.2500 0.0595(4) Uani 1 2 d S . .
Br2 Br 0.9647(3) 0.3197(12) 0.8623(3) 0.164(3) Uani 0.440(9) 1 d P . .
N1 N 0.5912(4) 0.7365(7) 1.1760(4) 0.0444(13) Uani 1 1 d . . .
C2 C 0.5446(5) 0.7494(8) 1.0816(4) 0.0447(16) Uani 1 1 d . . .
C3 C 0.5958(5) 0.8195(9) 1.0181(5) 0.0464(16) Uani 1 1 d . . .
H3 H 0.564(5) 0.832(9) 0.953(5) 0.046(17) Uiso 1 1 d . . .
C4 C 0.6969(6) 0.8763(9) 1.0508(5) 0.0495(17) Uani 1 1 d . . .
C5 C 0.7412(6) 0.8701(10) 1.1484(6) 0.0577(18) Uani 1 1 d . . .
H5 H 0.806(6) 0.897(9) 1.172(5) 0.06(2) Uiso 1 1 d . . .
C6 C 0.6874(6) 0.7991(10) 1.2078(5) 0.0558(18) Uani 1 1 d . . .
H6 H 0.712(4) 0.785(6) 1.275(4) 0.022(13) Uiso 1 1 d . . .
C7 C 0.7541(8) 0.9412(15) 0.9812(8) 0.071(2) Uani 1 1 d . . .
H7A H 0.795(7) 1.019(12) 1.006(6) 0.07(3) Uiso 1 1 d . . .
H7C H 0.711(6) 0.927(10) 0.916(6) 0.08(3) Uiso 1 1 d . . .
H7B H 0.816(10) 0.889(17) 0.987(9) 0.15(5) Uiso 1 1 d . . .
N1' N 0.4019(4) 0.6093(7) 1.1205(4) 0.0457(13) Uani 1 1 d . . .
C2' C 0.4372(5) 0.6801(8) 1.0488(4) 0.0420(15) Uani 1 1 d . . .
C3' C 0.3758(5) 0.6846(9) 0.9555(4) 0.0451(16) Uani 1 1 d . . .
H3' H 0.404(5) 0.730(7) 0.907(5) 0.044(17) Uiso 1 1 d . . .
C4' C 0.2761(5) 0.6217(9) 0.9313(4) 0.0459(16) Uani 1 1 d . . .
C5' C 0.2419(6) 0.5463(10) 1.0044(5) 0.0550(17) Uani 1 1 d . . .
H5' H 0.174(5) 0.515(8) 0.994(4) 0.044(18) Uiso 1 1 d . . .
C6' C 0.3053(6) 0.5425(10) 1.0956(5) 0.0529(18) Uani 1 1 d . . .
H6' H 0.293(5) 0.501(9) 1.146(5) 0.047(18) Uiso 1 1 d . . .
C7' C 0.2077(9) 0.6310(16) 0.8304(6) 0.072(3) Uani 1 1 d . . .
H7'A H 0.207(8) 0.519(16) 0.801(8) 0.13(4) Uiso 1 1 d . . .
H7'B H 0.241(6) 0.702(11) 0.793(6) 0.08(3) Uiso 1 1 d . . .
H7'C H 0.168(6) 0.706(12) 0.831(6) 0.07(3) Uiso 1 1 d . . .
O1 O 0.964(2) 0.735(5) 0.9028(17) 0.160(16) Uani 0.58(4) 1 d P . .
O2 O 0.9665(15) 0.198(4) 0.8821(17) 0.173(15) Uani 0.560(9) 1 d P . .
O3 O 1.0000 1.0000 1.0000 0.21(2) Uani 0.52(3) 2 d SP . .
O4 O 0.974(2) 0.649(6) 0.930(3) 0.20(2) Uani 0.42(4) 1 d P . .
O5 O 0.9799(17) 0.966(4) 0.818(4) 0.26(2) Uani 0.58(4) 1 d P . .
O6 O 0.9693(19) 0.843(6) 0.8779(17) 0.112(17) Uani 0.42(4) 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1' Cu1 N1' 177.2(3) . 2_657 ?
N1' Cu1 N1 98.3(2) . 2_657 ?
N1' Cu1 N1 80.4(2) 2_657 2_657 ?
N1' Cu1 N1 80.4(2) . . ?
N1' Cu1 N1 98.3(2) 2_657 . ?
N1 Cu1 N1 122.7(3) 2_657 . ?
N1' Cu1 Br1 91.39(15) . . ?
N1' Cu1 Br1 91.39(15) 2_657 . ?
N1 Cu1 Br1 118.66(14) 2_657 . ?
N1 Cu1 Br1 118.66(14) . . ?
C6 N1 C2 117.7(6) . . ?
C6 N1 Cu1 129.7(5) . . ?
C2 N1 Cu1 112.4(4) . . ?
N1 C2 C3 121.5(6) . . ?
N1 C2 C2' 116.3(5) . . ?
C3 C2 C2' 122.2(6) . . ?
C4 C3 C2 120.5(6) . . ?
C5 C4 C3 116.8(6) . . ?
C5 C4 C7 122.9(8) . . ?
C3 C4 C7 120.3(7) . . ?
C6 C5 C4 120.3(7) . . ?
N1 C6 C5 123.1(7) . . ?
C6' N1' C2' 116.9(5) . . ?
C6' N1' Cu1 126.1(4) . . ?
C2' N1' Cu1 116.9(4) . . ?
N1' C2' C3' 121.2(6) . . ?
N1' C2' C2 113.7(5) . . ?
C3' C2' C2 125.1(6) . . ?
C4' C3' C2' 121.6(6) . . ?
C3' C4' C5' 116.7(6) . . ?
C3' C4' C7' 121.9(7) . . ?
C5' C4' C7' 121.5(8) . . ?
C6' C5' C4' 120.0(7) . . ?
N1' C6' C5' 123.6(7) . . ?
O4 O1 O6 164(6) . . ?
O1 O4 O6 9(4) . . ?
O1 O6 O5 161(4) . . ?
O1 O6 O4 7(3) . . ?
O5 O6 O4 161(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1' 1.971(5) . ?
Cu1 N1' 1.971(5) 2_657 ?
Cu1 N1 2.085(5) 2_657 ?
Cu1 N1 2.085(5) . ?
Cu1 Br1 2.5150(16) . ?
Br2 O2 0.96(2) . ?
N1 C6 1.330(8) . ?
N1 C2 1.340(8) . ?
C2 C3 1.389(9) . ?
C2 C2' 1.480(9) . ?
C3 C4 1.374(9) . ?
C4 C5 1.374(10) . ?
C4 C7 1.501(10) . ?
C5 C6 1.369(10) . ?
N1' C6' 1.341(9) . ?
N1' C2' 1.359(8) . ?
C2' C3' 1.374(8) . ?
C3' C4' 1.368(9) . ?
C4' C5' 1.382(10) . ?
C4' C7' 1.497(10) . ?
C5' C6' 1.359(10) . ?
O1 O4 0.75(4) . ?
O1 O6 0.90(4) . ?
O4 O6 1.63(5) . ?
O5 O6 1.30(4) . ?
