#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:42:30 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178610 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/21/4072164.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_4072164
loop_
_publ_author_name
'Wolf, Joffrey'
'Poli, Rinaldo'
'Xie, Jian-Hua'
'Nichols, Jason'
'Xi, Bin'
'Zavalij, Peter'
'Doyle, Michael P.'
_publ_section_title
;
 Removal of Metal−Metal Bonding in a Dimetallic Paddlewheel
 Complex: Molecular and Electronic Structure of Bis(phenyl) Dirhodium(III)
 Carboxamidate Compounds
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5836
_journal_paper_doi               10.1021/om800631b
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C20 H36 N4 O6 Rh2, B F4'
_chemical_formula_sum            'C20 H36 B F4 N4 O6 Rh2'
_chemical_formula_weight         721.16
_chemical_name_systematic
; 
Tetrakis-μ-(valerolactamate)-bis(hydrate)dirhodium(II,III) tetrafluoroborate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.8230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4694(6)
_cell_length_b                   17.4131(8)
_cell_length_c                   13.4049(6)
_cell_measurement_reflns_used    6023
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.2
_cell_volume                     2720.5(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      606,606,606
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0735341
_diffrn_orient_matrix_UB_12      -0.0292911
_diffrn_orient_matrix_UB_13      0.0188893
_diffrn_orient_matrix_UB_21      0.0434919
_diffrn_orient_matrix_UB_22      0.0464791
_diffrn_orient_matrix_UB_23      0.0365240
_diffrn_orient_matrix_UB_31      -0.0079399
_diffrn_orient_matrix_UB_32      -0.0167251
_diffrn_orient_matrix_UB_33      0.0684057
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11969
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       needle
_exptl_crystal_F_000             1452
_exptl_crystal_id                'Doyle/Wolf WJ482(2)'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.01P)²+8.84P], P=(max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                2719
_reflns_number_total             3122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800631b_si_002.cif
_cod_data_source_block           2b'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4072164
#BEGIN Tags that were not found in dictionaries:
_diffrn_measurement_total_frames-ccd 1818
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.940
_diffrn_measurement_frame_time-ccd 33
_diffrn_measurement_total_time-ccd 20.28
_diffrn_measurement_frame_size-ccd 512
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.538346(15) 0.045836(10) 0.569876(13) 0.02223(6) Uani 1 1 d .
O1 O 0.60785(14) -0.03991(9) 0.39775(12) 0.0257(3) Uani 1 1 d .
N1 N 0.68152(17) 0.04506(11) 0.53393(15) 0.0264(4) Uani 1 1 d .
C11 C 0.6898(2) 0.00443(13) 0.45503(18) 0.0259(5) Uani 1 1 d .
C12 C 0.7946(2) 0.00492(16) 0.4237(2) 0.0340(6) Uani 1 1 d .
H12A H 0.7702 0.0111 0.3461 0.050(9) Uiso 1 1 calc R
H12B H 0.8334 -0.0448 0.4422 0.047(9) Uiso 1 1 calc R
C13 C 0.8792(2) 0.06798(18) 0.4771(2) 0.0431(7) Uani 1 1 d .
H13A H 0.9530 0.0577 0.4693 0.046(8) Uiso 1 1 calc R
H13B H 0.8504 0.1175 0.4434 0.071(11) Uiso 1 1 calc R
C14 C 0.8942(3) 0.0707(2) 0.5927(2) 0.0481(7) Uani 1 1 d .
H14A H 0.9519 0.1094 0.6293 0.064(10) Uiso 1 1 calc R
H14B H 0.9208 0.0207 0.6259 0.067(11) Uiso 1 1 calc R
C15 C 0.7789(2) 0.09100(18) 0.6033(2) 0.0430(7) Uani 1 1 d .
H15A H 0.7855 0.0836 0.6777 0.058(10) Uiso 1 1 calc R
H15B H 0.7628 0.1455 0.5860 0.039(8) Uiso 1 1 calc R
O2 O 0.39835(14) 0.04064(9) 0.32593(13) 0.0270(3) Uani 1 1 d .
N2 N 0.46417(17) 0.12773(11) 0.46088(16) 0.0275(4) Uani 1 1 d .
C21 C 0.4085(2) 0.11018(13) 0.36139(18) 0.0275(5) Uani 1 1 d .
C22 C 0.3524(2) 0.16895(15) 0.2773(2) 0.0373(6) Uani 1 1 d .
H22A H 0.2692 0.1614 0.2521 0.042(8) Uiso 1 1 calc R
H22B H 0.3773 0.1605 0.2166 0.046(8) Uiso 1 1 calc R
C23 C 0.3793(3) 0.25127(17) 0.3152(2) 0.0532(8) Uani 1 1 d .
H23A H 0.4558 0.2654 0.3164 0.058(10) Uiso 1 1 calc R
H23B H 0.3232 0.2861 0.2663 0.068(11) Uiso 1 1 calc R
C24 C 0.3747(3) 0.25809(18) 0.4245(2) 0.0550(9) Uani 1 1 d .
H24A H 0.2981 0.2437 0.4228 0.069(12) Uiso 1 1 calc R
H24B H 0.3890 0.3115 0.4487 0.072(11) Uiso 1 1 calc R
C25 C 0.4639(3) 0.20626(15) 0.5020(2) 0.0446(7) Uani 1 1 d .
H25A H 0.5400 0.2290 0.5177 0.039(8) Uiso 1 1 calc R
H25B H 0.4491 0.2036 0.5690 0.047(9) Uiso 1 1 calc R
O3 O 0.61446(16) 0.12083(10) 0.72055(13) 0.0313(4) Uani 1 1 d D
H31 H 0.613(3) 0.0895(14) 0.770(2) 0.074(12) Uiso 1 1 d D
H32 H 0.602(2) 0.1693(6) 0.723(2) 0.041(8) Uiso 1 1 d D
B1 B 0.5000 0.3251(2) 0.7500 0.0475(11) Uani 1 2 d SDU
F1 F 0.5425(15) 0.3606(9) 0.8455(10) 0.108(5) Uani 0.50 1 d PDU
F2 F 0.5852(7) 0.2818(8) 0.7334(12) 0.063(2) Uani 0.50 1 d PDU
F3 F 0.4549(11) 0.3761(9) 0.6697(10) 0.095(4) Uani 0.50 1 d PDU
F4 F 0.4175(10) 0.2729(8) 0.7512(14) 0.087(4) Uani 0.50 1 d PDU
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
N1 Rh1 O2 89.93(7) . 5_656
N1 Rh1 N2 92.80(8) . .
O2 Rh1 N2 175.71(7) 5_656 .
N1 Rh1 O1 176.42(7) . 5_656
O2 Rh1 O1 88.51(7) 5_656 5_656
N2 Rh1 O1 88.58(7) . 5_656
N1 Rh1 O3 95.15(7) . .
O2 Rh1 O3 83.01(6) 5_656 .
N2 Rh1 O3 100.03(7) . .
O1 Rh1 O3 87.86(6) 5_656 .
N1 Rh1 Rh1 87.11(5) . 5_656
O2 Rh1 Rh1 89.61(5) 5_656 5_656
N2 Rh1 Rh1 87.23(5) . 5_656
O1 Rh1 Rh1 89.66(4) 5_656 5_656
O3 Rh1 Rh1 172.27(5) . 5_656
C11 O1 Rh1 119.08(14) . 5_656
C11 N1 C15 121.3(2) . .
C11 N1 Rh1 122.07(16) . .
C15 N1 Rh1 116.64(15) . .
O1 C11 N1 122.0(2) . .
O1 C11 C12 114.7(2) . .
N1 C11 C12 123.2(2) . .
C11 C12 C13 113.5(2) . .
C11 C12 H12A 108.9 . .
C13 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
C13 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
C14 C13 C12 108.8(2) . .
C14 C13 H13A 109.9 . .
C12 C13 H13A 109.9 . .
C14 C13 H13B 109.9 . .
C12 C13 H13B 109.9 . .
H13A C13 H13B 108.3 . .
C13 C14 C15 109.1(2) . .
C13 C14 H14A 109.9 . .
C15 C14 H14A 109.9 . .
C13 C14 H14B 109.9 . .
C15 C14 H14B 109.9 . .
H14A C14 H14B 108.3 . .
N1 C15 C14 113.9(2) . .
N1 C15 H15A 108.8 . .
C14 C15 H15A 108.8 . .
N1 C15 H15B 108.8 . .
C14 C15 H15B 108.8 . .
H15A C15 H15B 107.7 . .
C21 O2 Rh1 118.89(14) . 5_656
C21 N2 C25 121.9(2) . .
C21 N2 Rh1 121.10(16) . .
C25 N2 Rh1 116.53(16) . .
O2 C21 N2 123.0(2) . .
O2 C21 C22 113.9(2) . .
N2 C21 C22 123.1(2) . .
C21 C22 C23 113.9(2) . .
C21 C22 H22A 108.8 . .
C23 C22 H22A 108.8 . .
C21 C22 H22B 108.8 . .
C23 C22 H22B 108.8 . .
H22A C22 H22B 107.7 . .
C24 C23 C22 108.8(3) . .
C24 C23 H23A 109.9 . .
C22 C23 H23A 109.9 . .
C24 C23 H23B 109.9 . .
C22 C23 H23B 109.9 . .
H23A C23 H23B 108.3 . .
C23 C24 C25 110.5(3) . .
C23 C24 H24A 109.6 . .
C25 C24 H24A 109.6 . .
C23 C24 H24B 109.6 . .
C25 C24 H24B 109.6 . .
H24A C24 H24B 108.1 . .
N2 C25 C24 113.2(2) . .
N2 C25 H25A 108.9 . .
C24 C25 H25A 108.9 . .
N2 C25 H25B 108.9 . .
C24 C25 H25B 108.9 . .
H25A C25 H25B 107.8 . .
Rh1 O3 H31 102(2) . .
Rh1 O3 H32 124.3(19) . .
H31 O3 H32 122(2) . .
F1 B1 F3 111.4(5) . .
F1 B1 F4 109.5(9) . .
F3 B1 F4 109.9(8) . .
F1 B1 F2 109.7(9) . .
F3 B1 F2 110.8(9) . .
F4 B1 F2 105.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 2.0078(19) .
Rh1 O2 2.0143(16) 5_656
Rh1 N2 2.016(2) .
Rh1 O1 2.0211(16) 5_656
Rh1 O3 2.3071(16) .
Rh1 Rh1 2.3872(3) 5_656
O1 C11 1.293(3) .
O1 Rh1 2.0210(16) 5_656
N1 C11 1.307(3) .
N1 C15 1.475(3) .
C11 C12 1.507(3) .
C12 C13 1.515(4) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C13 C14 1.493(4) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C14 C15 1.535(4) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
O2 C21 1.291(3) .
O2 Rh1 2.0143(16) 5_656
N2 C21 1.302(3) .
N2 C25 1.475(3) .
C21 C22 1.499(3) .
C22 C23 1.518(4) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C23 C24 1.491(4) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C24 C25 1.519(4) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
O3 H31 0.862(10) .
O3 H32 0.861(10) .
B1 F1 1.349(8) .
B1 F3 1.354(7) .
B1 F4 1.377(7) .
B1 F2 1.384(7) .
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
O3 H31 O1 0.862(10) 1.941(13) 2.788(2) 167(3) 6_556
O3 H32 F4 0.861(10) 1.869(16) 2.725(12) 172(3) 2_656
O3 H32 F2 0.861(10) 1.981(16) 2.840(12) 176(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O2 Rh1 N1 C11 92.23(19) 5_656
N2 Rh1 N1 C11 -84.47(19) .
O3 Rh1 N1 C11 175.20(18) .
Rh1 Rh1 N1 C11 2.61(18) 5_656
O2 Rh1 N1 C15 -85.96(19) 5_656
N2 Rh1 N1 C15 97.3(2) .
O3 Rh1 N1 C15 -3.0(2) .
Rh1 Rh1 N1 C15 -175.58(19) 5_656
Rh1 O1 C11 N1 0.6(3) 5_656
Rh1 O1 C11 C12 -179.64(15) 5_656
C15 N1 C11 O1 175.5(2) .
Rh1 N1 C11 O1 -2.6(3) .
C15 N1 C11 C12 -4.2(4) .
Rh1 N1 C11 C12 177.73(18) .
O1 C11 C12 C13 168.9(2) .
N1 C11 C12 C13 -11.4(4) .
C11 C12 C13 C14 44.8(3) .
C12 C13 C14 C15 -62.5(3) .
C11 N1 C15 C14 -14.6(4) .
Rh1 N1 C15 C14 163.6(2) .
C13 C14 C15 N1 48.3(4) .
N1 Rh1 N2 C21 84.83(19) .
O1 Rh1 N2 C21 -91.86(19) 5_656
O3 Rh1 N2 C21 -179.44(18) .
Rh1 Rh1 N2 C21 -2.13(18) 5_656
N1 Rh1 N2 C25 -102.6(2) .
O1 Rh1 N2 C25 80.7(2) 5_656
O3 Rh1 N2 C25 -6.8(2) .
Rh1 Rh1 N2 C25 170.47(19) 5_656
Rh1 O2 C21 N2 4.4(3) 5_656
Rh1 O2 C21 C22 -176.77(16) 5_656
C25 N2 C21 O2 -173.1(2) .
Rh1 N2 C21 O2 -0.9(3) .
C25 N2 C21 C22 8.1(4) .
Rh1 N2 C21 C22 -179.68(19) .
O2 C21 C22 C23 -171.3(2) .
N2 C21 C22 C23 7.5(4) .
C21 C22 C23 C24 -41.8(4) .
C22 C23 C24 C25 61.4(4) .
C21 N2 C25 C24 12.0(4) .
Rh1 N2 C25 C24 -160.6(2) .
C23 C24 C25 N2 -47.2(4) .
