#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:58:58 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179549 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/18/4501880.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_4501880
loop_
_publ_author_name
'Laurila, Elina'
'Oresmaa, Larisa'
'Niskanen, Mika'
'Hirva, Pipsa'
'Haukka, Matti'
_publ_section_title
;
 Metal−Metal Interactions in Stacked Mononuclear and Dinuclear
 Rhodium 2,2′-Biimidazole Carbonyl Complexes
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3775
_journal_paper_doi               10.1021/cg100606f
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C8 H6 N4 O2 Rh, B F4'
_chemical_formula_sum            'C8 H6 B F4 N4 O2 Rh'
_chemical_formula_weight         379.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.8558(9)
_cell_length_b                   6.5035(4)
_cell_length_c                   20.0646(13)
_cell_measurement_reflns_used    7465
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.28
_cell_volume                     2330.0(2)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.3.2c (Brandenburg, 2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'62mm x 62mm CCD camera on three-circle goniostat'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ scans and ω scans'
_diffrn_radiation_monochromator  'flat graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29546
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_correction_T_min  0.7979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'metallic brownish'
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0271
_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/[σ²(Fo²)+(0.0335P)²+0.8760P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                2838
_reflns_number_total             3568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100606f_si_002.cif
_cod_data_source_block           3
_cod_database_code               4501880
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, 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
Rh1 Rh 0.739853(9) 0.13361(2) 0.031471(8) 0.01399(6) Uani 1 1 d .
F1 F 0.96842(9) 0.2103(2) 0.38703(8) 0.0378(4) Uani 1 1 d .
F2 F 0.89425(8) 0.2701(2) 0.29674(7) 0.0298(3) Uani 1 1 d .
F3 F 0.87453(9) -0.0106(3) 0.36124(8) 0.0407(4) Uani 1 1 d .
F4 F 0.97684(8) 0.0095(2) 0.29467(8) 0.0381(4) Uani 1 1 d .
O1 O 0.78645(10) 0.0577(3) -0.10987(9) 0.0308(4) Uani 1 1 d .
O2 O 0.57638(9) 0.1380(2) -0.00270(9) 0.0280(4) Uani 1 1 d .
N1 N 0.71606(10) 0.1658(2) 0.13225(9) 0.0152(3) Uani 1 1 d .
H1N H 0.9325 0.2079 0.2022 0.023 Uiso 1 1 d R
N2 N 0.75785(10) 0.2052(3) 0.23452(10) 0.0179(4) Uani 1 1 d .
H2N H 0.7865 0.2108 0.2653 0.027 Uiso 1 1 d R
N3 N 0.84733(9) 0.1465(2) 0.07139(9) 0.0150(3) Uani 1 1 d .
N4 N 0.91903(10) 0.1864(3) 0.15930(9) 0.0181(4) Uani 1 1 d .
C1 C 0.76864(12) 0.0899(3) -0.05680(13) 0.0200(4) Uani 1 1 d .
C2 C 0.63866(13) 0.1321(3) 0.00787(12) 0.0187(4) Uani 1 1 d .
C5 C 0.65552(11) 0.1808(3) 0.17481(12) 0.0181(4) Uani 1 1 d .
H5 H 0.6044 0.1753 0.1619 0.022 Uiso 1 1 calc R
C6 C 0.68076(12) 0.2047(3) 0.23785(12) 0.0202(4) Uani 1 1 d .
H6 H 0.6511 0.2185 0.2769 0.024 Uiso 1 1 calc R
C8 C 0.77693(11) 0.1813(3) 0.17053(11) 0.0146(4) Uani 1 1 d .
C9 C 0.84840(11) 0.1712(3) 0.13712(11) 0.0137(4) Uani 1 1 d .
C11 C 0.96550(12) 0.1729(3) 0.10491(12) 0.0208(4) Uani 1 1 d .
H11 H 1.0186 0.1800 0.1052 0.025 Uiso 1 1 calc R
C12 C 0.92091(12) 0.1475(3) 0.05076(12) 0.0179(4) Uani 1 1 d .
H12 H 0.9376 0.1329 0.0061 0.022 Uiso 1 1 calc R
B1 B 0.92931(14) 0.1184(4) 0.33652(14) 0.0209(5) Uani 1 1 d .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 '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
C1 Rh1 C2 91.43(10) . . yes
C1 Rh1 N1 174.78(8) . . ?
C2 Rh1 N1 92.84(9) . . ?
C1 Rh1 N3 96.74(8) . . ?
C2 Rh1 N3 171.79(9) . . ?
N1 Rh1 N3 79.04(7) . . yes
C1 Rh1 Rh1 96.94(7) . 7_765 ?
C2 Rh1 Rh1 96.44(6) . 7_765 ?
N1 Rh1 Rh1 85.56(4) . 7_765 ?
N3 Rh1 Rh1 81.83(4) . 7_765 ?
C1 Rh1 Rh1 79.53(7) . 7_755 ?
C2 Rh1 Rh1 95.86(6) . 7_755 ?
N1 Rh1 Rh1 97.05(4) . 7_755 ?
N3 Rh1 Rh1 86.44(4) . 7_755 ?
Rh1 Rh1 Rh1 167.283(11) 7_765 7_755 yes
C8 N1 C5 106.03(18) . . ?
C8 N1 Rh1 113.67(14) . . ?
C5 N1 Rh1 140.29(15) . . ?
C8 N2 C6 107.50(19) . . ?
C8 N2 H2N 125.6 . . ?
C6 N2 H2N 126.8 . . ?
C9 N3 C12 106.50(18) . . ?
C9 N3 Rh1 113.58(13) . . ?
C12 N3 Rh1 139.82(16) . . ?
C9 N4 C11 107.44(18) . . ?
C9 N4 H1N 125.3 . . ?
C11 N4 H1N 127.2 . . ?
O1 C1 Rh1 178.0(2) . . ?
O2 C2 Rh1 175.5(2) . . ?
C6 C5 N1 109.01(19) . . ?
C6 C5 H5 125.5 . . ?
N1 C5 H5 125.5 . . ?
C5 C6 N2 106.7(2) . . ?
C5 C6 H6 126.6 . . ?
N2 C6 H6 126.6 . . ?
N1 C8 N2 110.73(18) . . ?
N1 C8 C9 116.69(19) . . ?
N2 C8 C9 132.6(2) . . ?
N3 C9 N4 110.60(18) . . ?
N3 C9 C8 117.00(18) . . ?
N4 C9 C8 132.4(2) . . ?
C12 C11 N4 106.81(19) . . ?
C12 C11 H11 126.6 . . ?
N4 C11 H11 126.6 . . ?
C11 C12 N3 108.6(2) . . ?
C11 C12 H12 125.7 . . ?
N3 C12 H12 125.7 . . ?
F1 B1 F3 111.2(2) . . ?
F1 B1 F4 111.0(2) . . ?
F3 B1 F4 109.9(2) . . ?
F1 B1 F2 109.82(19) . . ?
F3 B1 F2 108.23(19) . . ?
F4 B1 F2 106.6(2) . . ?
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
Rh1 C1 1.866(3) . yes
Rh1 C2 1.868(2) . yes
Rh1 N1 2.0767(18) . yes
Rh1 N3 2.0813(17) . yes
Rh1 Rh1 3.2719(2) 7_765 yes
Rh1 Rh1 3.2719(2) 7_755 yes
F1 B1 1.368(3) . ?
F2 B1 1.415(3) . ?
F3 B1 1.381(3) . ?
F4 B1 1.388(3) . ?
O1 C1 1.131(3) . ?
O2 C2 1.133(3) . ?
N1 C8 1.335(3) . ?
N1 C5 1.381(3) . ?
N2 C8 1.337(3) . ?
N2 C6 1.378(3) . ?
N2 H2N 0.8029 . ?
N3 C9 1.329(3) . ?
N3 C12 1.377(3) . ?
N4 C9 1.341(3) . ?
N4 C11 1.374(3) . ?
N4 H1N 0.9053 . ?
C5 C6 1.352(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.443(3) . ?
C11 C12 1.357(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N4 H1N F2 0.91 2.06 2.845(2) 145.0 yes
N4 H1N F4 0.91 2.39 3.125(2) 137.9 yes
N2 H2N F2 0.80 2.06 2.769(2) 147.0 yes
