#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:58:58 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179549 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/18/4501878.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_4501878
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, N O3'
_chemical_formula_sum            'C8 H6 N5 O5 Rh'
_chemical_formula_weight         355.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.639(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.459(3)
_cell_length_b                   17.177(5)
_cell_length_c                   6.4473(18)
_cell_measurement_reflns_used    3208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.80
_cell_measurement_theta_min      2.35
_cell_volume                     1109.8(6)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7051
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.9119
_exptl_absorpt_correction_T_min  0.7766
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'metallic reddish'
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0173P)²+1.7448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                2040
_reflns_number_total             2550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100606f_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        1109.8(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4501878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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 0.56161(3) 0.241154(14) 0.42033(4) 0.01288(8) Uani 1 1 d .
O1 O 0.2835(3) 0.30177(16) 0.3384(5) 0.0323(7) Uani 1 1 d .
O2 O 0.4783(3) 0.07426(15) 0.3625(5) 0.0299(7) Uani 1 1 d .
O3 O 0.1770(3) 0.14076(18) 0.3145(6) 0.0465(9) Uani 1 1 d .
O4 O 0.0783(3) 0.03061(17) 0.2742(6) 0.0455(9) Uani 1 1 d .
O5 O 0.2486(3) 0.04928(18) 0.5467(5) 0.0384(8) Uani 1 1 d .
N1 N 0.7633(3) 0.21267(15) 0.5241(4) 0.0137(6) Uani 1 1 d .
N2 N 0.9707(3) 0.25250(17) 0.6581(4) 0.0161(6) Uani 1 1 d .
H2N H 1.039(5) 0.287(3) 0.703(8) 0.043(14) Uiso 1 1 d .
N3 N 0.6480(3) 0.35045(16) 0.4591(4) 0.0142(6) Uani 1 1 d .
N4 N 0.8291(3) 0.42220(16) 0.5654(5) 0.0167(6) Uani 1 1 d .
H4N H 0.910(4) 0.435(2) 0.616(7) 0.024(12) Uiso 1 1 d .
N5 N 0.1688(3) 0.07431(18) 0.3800(5) 0.0243(7) Uani 1 1 d .
C1 C 0.3880(4) 0.27734(19) 0.3620(6) 0.0201(8) Uani 1 1 d .
C2 C 0.5055(4) 0.1378(2) 0.3863(6) 0.0184(7) Uani 1 1 d .
C5 C 0.8439(4) 0.14820(19) 0.5722(5) 0.0158(7) Uani 1 1 d .
H5 H 0.8148 0.0956 0.5510 0.019 Uiso 1 1 calc R
C6 C 0.9723(4) 0.17221(19) 0.6553(5) 0.0160(7) Uani 1 1 d .
H6 H 1.0487 0.1398 0.7026 0.019 Uiso 1 1 calc R
C8 C 0.8425(3) 0.27454(18) 0.5778(5) 0.0131(7) Uani 1 1 d .
C9 C 0.7797(4) 0.34981(19) 0.5404(5) 0.0149(7) Uani 1 1 d .
C11 C 0.7232(4) 0.4715(2) 0.4944(6) 0.0205(8) Uani 1 1 d .
H11 H 0.7272 0.5268 0.4922 0.025 Uiso 1 1 calc R
C12 C 0.6118(4) 0.42774(19) 0.4279(6) 0.0183(7) Uani 1 1 d .
H12 H 0.5236 0.4469 0.3696 0.022 Uiso 1 1 calc R
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'
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 92.20(16) . . yes
C1 Rh1 N3 95.09(13) . . ?
C2 Rh1 N3 172.60(14) . . ?
C1 Rh1 N1 171.31(13) . . ?
C2 Rh1 N1 94.01(14) . . ?
N3 Rh1 N1 78.88(11) . . yes
C1 Rh1 Rh1 83.75(11) . 4_566 ?
C2 Rh1 Rh1 96.71(11) . 4_566 ?
N3 Rh1 Rh1 85.36(8) . 4_566 ?
N1 Rh1 Rh1 89.49(7) . 4_566 ?
C1 Rh1 Rh1 92.63(11) . 4_565 ?
C2 Rh1 Rh1 93.56(11) . 4_565 ?
N3 Rh1 Rh1 84.86(8) . 4_565 ?
N1 Rh1 Rh1 93.04(7) . 4_565 ?
Rh1 Rh1 Rh1 169.230(17) 4_566 4_565 yes
C8 N1 C5 106.8(3) . . ?
C8 N1 Rh1 113.2(2) . . ?
C5 N1 Rh1 139.7(2) . . ?
C8 N2 C6 106.9(3) . . ?
C8 N2 H2N 123(3) . . ?
C6 N2 H2N 130(3) . . ?
C9 N3 C12 106.0(3) . . ?
C9 N3 Rh1 114.1(2) . . ?
C12 N3 Rh1 139.9(3) . . ?
C9 N4 C11 106.7(3) . . ?
C9 N4 H4N 127(3) . . ?
C11 N4 H4N 127(3) . . ?
O3 N5 O5 121.8(4) . . ?
O3 N5 O4 119.2(4) . . ?
O5 N5 O4 119.0(3) . . ?
O1 C1 Rh1 175.8(3) . . ?
O2 C2 Rh1 175.9(3) . . ?
C6 C5 N1 108.5(3) . . ?
C6 C5 H5 125.7 . . ?
N1 C5 H5 125.7 . . ?
C5 C6 N2 107.1(3) . . ?
C5 C6 H6 126.4 . . ?
N2 C6 H6 126.4 . . ?
N1 C8 N2 110.7(3) . . ?
N1 C8 C9 117.0(3) . . ?
N2 C8 C9 132.4(3) . . ?
N3 C9 N4 111.2(3) . . ?
N3 C9 C8 116.5(3) . . ?
N4 C9 C8 132.3(4) . . ?
C12 C11 N4 107.7(3) . . ?
C12 C11 H11 126.1 . . ?
N4 C11 H11 126.1 . . ?
C11 C12 N3 108.3(3) . . ?
C11 C12 H12 125.8 . . ?
N3 C12 H12 125.8 . . ?
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 1.853(4) . yes
Rh1 C2 1.863(4) . yes
Rh1 N3 2.067(3) . yes
Rh1 N1 2.080(3) . yes
Rh1 Rh1 3.2379(9) 4_566 yes
Rh1 Rh1 3.2379(9) 4_565 yes
O1 C1 1.139(4) . ?
O2 C2 1.128(4) . ?
O3 N5 1.228(4) . ?
O4 N5 1.247(4) . ?
O5 N5 1.234(4) . ?
N1 C8 1.331(4) . ?
N1 C5 1.372(4) . ?
N2 C8 1.346(4) . ?
N2 C6 1.379(4) . ?
N2 H2N 0.91(5) . ?
N3 C9 1.327(5) . ?
N3 C12 1.379(4) . ?
N4 C9 1.339(4) . ?
N4 C11 1.365(5) . ?
N4 H4N 0.84(4) . ?
C5 C6 1.360(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.439(5) . ?
C11 C12 1.349(5) . ?
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_site_symmetry_A
_geom_hbond_publ_flag
N2 H2N O3 0.91(5) 1.88(5) 2.790(4) 175(4) 4_666 yes
N4 H4N O4 0.84(4) 1.86(4) 2.693(4) 169(4) 4_666 yes
