#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:58:58 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179549 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/18/4501881.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_4501881
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   geom
_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                   17.9281(5)
_cell_length_b                   6.5784(2)
_cell_length_c                   20.1763(5)
_cell_measurement_reflns_used    4977
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.32
_cell_volume                     2379.56(11)
_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      220(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26488
_diffrn_reflns_theta_full        35.32
_diffrn_reflns_theta_max         35.32
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.9144
_exptl_absorpt_correction_T_min  0.8015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'metallic brownish'
_exptl_crystal_density_diffrn    2.121
_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         1.071
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0357
_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)+(0.0296P)²+0.9792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                3384
_reflns_number_total             5353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100606f_si_002.cif
_cod_data_source_block           3B
_cod_database_code               4501881
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 0.739790(9) 0.12945(3) 0.032352(8) 0.02738(5) Uani 1 1 d .
F1 F 0.96336(13) 0.2071(3) 0.38844(9) 0.0856(7) Uani 1 1 d .
F2 F 0.89424(11) 0.2634(3) 0.29694(9) 0.0718(6) Uani 1 1 d .
F3 F 0.87492(13) -0.0126(4) 0.35869(10) 0.0962(8) Uani 1 1 d .
F4 F 0.97691(11) 0.0155(4) 0.29726(11) 0.0871(7) Uani 1 1 d .
O1 O 0.78590(13) 0.0549(4) -0.10779(10) 0.0637(6) Uani 1 1 d .
O2 O 0.57782(11) 0.1374(3) -0.00257(11) 0.0565(6) Uani 1 1 d .
N1 N 0.71620(10) 0.1597(3) 0.13249(9) 0.0280(4) Uani 1 1 d .
H1N H 0.9327 0.2018 0.2025 0.042 Uiso 1 1 d R
N2 N 0.75778(11) 0.1931(3) 0.23442(10) 0.0336(4) Uani 1 1 d .
H2N H 0.7864 0.1987 0.2652 0.050 Uiso 1 1 d R
N3 N 0.84682(10) 0.1419(3) 0.07195(9) 0.0275(4) Uani 1 1 d .
N4 N 0.91789(11) 0.1768(3) 0.15952(10) 0.0347(4) Uani 1 1 d .
C1 C 0.76852(15) 0.0872(4) -0.05521(14) 0.0403(6) Uani 1 1 d .
C2 C 0.63952(14) 0.1299(4) 0.00851(12) 0.0357(5) Uani 1 1 d .
C5 C 0.65597(13) 0.1726(3) 0.17490(13) 0.0335(5) Uani 1 1 d .
H5 H 0.6055 0.1681 0.1623 0.040 Uiso 1 1 calc R
C6 C 0.68150(14) 0.1926(4) 0.23731(13) 0.0383(5) Uani 1 1 d .
H6 H 0.6523 0.2040 0.2758 0.046 Uiso 1 1 calc R
C8 C 0.77689(12) 0.1722(3) 0.17044(11) 0.0257(4) Uani 1 1 d .
C9 C 0.84788(12) 0.1633(3) 0.13736(11) 0.0262(4) Uani 1 1 d .
C11 C 0.96407(13) 0.1645(4) 0.10551(13) 0.0398(6) Uani 1 1 d .
H11 H 1.0165 0.1700 0.1058 0.048 Uiso 1 1 calc R
C12 C 0.91983(13) 0.1431(4) 0.05167(12) 0.0351(5) Uani 1 1 d .
H12 H 0.9364 0.1309 0.0076 0.042 Uiso 1 1 calc R
B1 B 0.92783(16) 0.1190(5) 0.33712(15) 0.0423(7) 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
C2 Rh1 C1 91.27(11) . . yes
C2 Rh1 N1 93.13(9) . . ?
C1 Rh1 N1 174.63(9) . . ?
C2 Rh1 N3 172.02(9) . . ?
C1 Rh1 N3 96.62(10) . . ?
N1 Rh1 N3 79.05(7) . . yes
C2 Rh1 Rh1 96.03(8) . 7_765 ?
C1 Rh1 Rh1 96.77(8) . 7_765 ?
N1 Rh1 Rh1 85.82(5) . 7_765 ?
N3 Rh1 Rh1 81.88(5) . 7_765 ?
C2 Rh1 Rh1 96.23(7) . 7_755 ?
C1 Rh1 Rh1 79.69(8) . 7_755 ?
N1 Rh1 Rh1 96.77(5) . 7_755 ?
N3 Rh1 Rh1 86.40(5) . 7_755 ?
Rh1 Rh1 Rh1 167.299(11) 7_765 7_755 yes
C8 N1 C5 106.18(19) . . ?
C8 N1 Rh1 113.52(15) . . ?
C5 N1 Rh1 140.30(16) . . ?
C8 N2 C6 107.2(2) . . ?
C8 N2 H2N 125.6 . . ?
C6 N2 H2N 127.1 . . ?
C9 N3 C12 106.40(19) . . ?
C9 N3 Rh1 113.54(14) . . ?
C12 N3 Rh1 140.00(16) . . ?
C9 N4 C11 107.31(19) . . ?
C9 N4 H1N 126.7 . . ?
C11 N4 H1N 125.8 . . ?
O1 C1 Rh1 177.7(3) . . ?
O2 C2 Rh1 175.7(2) . . ?
C6 C5 N1 108.7(2) . . ?
C6 C5 H5 125.7 . . ?
N1 C5 H5 125.7 . . ?
C5 C6 N2 107.5(2) . . ?
C5 C6 H6 126.3 . . ?
N2 C6 H6 126.3 . . ?
N1 C8 N2 110.50(19) . . ?
N1 C8 C9 116.95(19) . . ?
N2 C8 C9 132.5(2) . . ?
N3 C9 N4 110.70(19) . . ?
N3 C9 C8 116.93(19) . . ?
N4 C9 C8 132.4(2) . . ?
C12 C11 N4 106.9(2) . . ?
C12 C11 H11 126.6 . . ?
N4 C11 H11 126.6 . . ?
C11 C12 N3 108.7(2) . . ?
C11 C12 H12 125.6 . . ?
N3 C12 H12 125.6 . . ?
F1 B1 F3 111.0(2) . . ?
F1 B1 F4 111.1(3) . . ?
F3 B1 F4 108.7(3) . . ?
F1 B1 F2 111.1(3) . . ?
F3 B1 F2 108.7(2) . . ?
F4 B1 F2 106.0(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 C2 1.861(2) . yes
Rh1 C1 1.861(3) . yes
Rh1 N1 2.0737(18) . yes
Rh1 N3 2.0801(18) . yes
Rh1 Rh1 3.3095(3) 7_765 yes
Rh1 Rh1 3.3095(3) 7_755 yes
F1 B1 1.347(3) . ?
F2 B1 1.386(3) . ?
F3 B1 1.356(4) . ?
F4 B1 1.373(4) . ?
O1 C1 1.126(3) . ?
O2 C2 1.130(3) . ?
N1 C8 1.333(3) . ?
N1 C5 1.380(3) . ?
N2 C8 1.343(3) . ?
N2 C6 1.369(3) . ?
N2 H2N 0.8069 . ?
N3 C9 1.327(3) . ?
N3 C12 1.371(3) . ?
N4 C9 1.335(3) . ?
N4 C11 1.371(3) . ?
N4 H1N 0.9211 . ?
C5 C6 1.346(4) . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
C8 C9 1.438(3) . ?
C11 C12 1.352(3) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
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 0.92 2.07 2.862(3) 143.8 yes
N4 H1N F4 0.92 2.41 3.157(3) 138.7 yes
N2 H2N F2 0.81 2.08 2.791(3) 146.9 yes
