#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/37/7003745.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_7003745
loop_
_publ_author_name
'Adams, Christopher J.'
'Anderson, Kirsty M.'
'Charmant, Jonathan P. H.'
'Connelly, Neil G.'
'Field, Bevis A.'
'Hallett, Andrew J.'
'Horne, Mathew'
_publ_section_title
;
 Solid state and solution structures of rhodium and iridium
 poly(pyrazolyl)borate diene complexes
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              2680
_journal_page_last               2692
_journal_paper_doi               10.1039/b719223a
_journal_year                    2008
_chemical_formula_sum            'C18 H23.5 B N6.5 Rh'
_chemical_formula_weight         444.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   10.8148(16)
_cell_length_b                   10.1274(14)
_cell_length_c                   33.316(5)
_cell_measurement_reflns_used    77
_cell_measurement_temperature    173(2)
_cell_volume                     3649.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens CCD area detector'
_diffrn_measurement_method       'ω scans with narrow frames'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            9597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.778369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0356
_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)+(0.0377P)²+3.9788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                2900
_reflns_number_total             3272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719223a.txt
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_original_formula_sum        'C18 H23.50 B N6.50 Rh'
_cod_database_code               7003745
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
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
Rh1 Rh 0.0000 0.60111(6) 0.418101(16) 0.01764(16) Uani 1 2 d S . .
B1 B 0.0000 0.3531(9) 0.3544(3) 0.019(2) Uani 1 2 d S . .
N5 N 0.0000 0.3961(7) 0.43007(18) 0.0210(16) Uani 1 2 d S . .
N6 N 0.0000 0.3068(6) 0.3989(2) 0.0161(16) Uani 1 2 d S . .
N1 N 0.1362(4) 0.5458(5) 0.36986(14) 0.0202(11) Uani 1 1 d . . .
N2 N 0.1153(4) 0.4361(4) 0.34712(13) 0.0182(10) Uani 1 1 d . . .
C10 C 0.0000 0.1842(10) 0.4143(4) 0.032(2) Uani 1 2 d S . .
H1A H 0.0000 0.1052 0.3989 0.038 Uiso 1 2 calc SR . .
C9 C 0.0000 0.1900(11) 0.4555(3) 0.040(3) Uani 1 2 d S . .
H2A H 0.0000 0.1188 0.4740 0.048 Uiso 1 2 calc SR . .
C8 C 0.0000 0.3273(9) 0.4637(3) 0.032(3) Uani 1 2 d S . .
H3A H 0.0000 0.3647 0.4898 0.038 Uiso 1 2 calc SR . .
C7 C 0.2084(6) 0.4190(6) 0.32050(18) 0.0234(14) Uani 1 1 d . . .
H4A H 0.2148 0.3497 0.3014 0.028 Uiso 1 1 calc R . .
C6 C 0.2924(6) 0.5200(6) 0.32601(19) 0.0288(15) Uani 1 1 d . . .
H5A H 0.3669 0.5353 0.3116 0.035 Uiso 1 1 calc R . .
C5 C 0.2432(6) 0.5948(6) 0.35747(19) 0.0236(16) Uani 1 1 d . . .
H6A H 0.2816 0.6709 0.3685 0.028 Uiso 1 1 calc R . .
C1 C 0.0634(5) 0.8004(5) 0.41030(18) 0.0254(15) Uani 1 1 d . . .
H7 H 0.0997 0.8168 0.3831 0.031 Uiso 1 1 calc R . .
C3 C 0.1453(6) 0.8459(6) 0.4438(2) 0.0357(16) Uani 1 1 d . . .
H8A H 0.2311 0.8520 0.4336 0.043 Uiso 1 1 calc R . .
H8B H 0.1194 0.9358 0.4518 0.043 Uiso 1 1 calc R . .
C2 C 0.1452(11) 0.7614(10) 0.4796(3) 0.090(4) Uani 1 1 d . . .
H9A H 0.1151 0.8134 0.5028 0.108 Uiso 1 1 calc R . .
H9B H 0.2312 0.7338 0.4855 0.108 Uiso 1 1 calc R . .
C4 C 0.0659(6) 0.6403(7) 0.47503(18) 0.0297(14) Uani 1 1 d . . .
H10 H 0.1019 0.5607 0.4884 0.036 Uiso 1 1 calc R . .
Rh11 Rh 0.0000 0.76338(5) 0.121394(17) 0.01749(16) Uani 1 2 d S . .
B11 B 0.0000 0.5115(9) 0.1837(3) 0.019(2) Uani 1 2 d S . .
N15 N 0.0000 0.5606(7) 0.10919(19) 0.0222(16) Uani 1 2 d SU . .
N16 N 0.0000 0.4714(7) 0.1392(2) 0.0185(18) Uani 1 2 d SU . .
N11 N 0.1352(4) 0.7071(5) 0.16957(14) 0.0205(10) Uani 1 1 d . . .
N12 N 0.1148(4) 0.5955(5) 0.19163(13) 0.0213(10) Uani 1 1 d . . .
C20 C 0.0000 0.3466(8) 0.1238(3) 0.0262(19) Uani 1 2 d S . .
H11A H 0.0000 0.2660 0.1384 0.031 Uiso 1 2 calc SR . .
C19 C 0.0000 0.3614(10) 0.0828(3) 0.041(3) Uani 1 2 d S . .
H12A H 0.0000 0.2920 0.0636 0.049 Uiso 1 2 calc SR . .
C18 C 0.0000 0.4904(11) 0.0747(3) 0.033(3) Uani 1 2 d SU . .
H13A H 0.0000 0.5275 0.0485 0.040 Uiso 1 2 calc SR . .
C17 C 0.2117(6) 0.5740(6) 0.21629(17) 0.0244(15) Uani 1 1 d . . .
H14A H 0.2205 0.5015 0.2342 0.029 Uiso 1 1 calc R . .
C16 C 0.2953(6) 0.6741(7) 0.2113(2) 0.0318(16) Uani 1 1 d . . .
H15A H 0.3716 0.6860 0.2249 0.038 Uiso 1 1 calc R . .
C15 C 0.2444(6) 0.7541(6) 0.1820(2) 0.0281(17) Uani 1 1 d . . .
H16A H 0.2820 0.8322 0.1720 0.034 Uiso 1 1 calc R . .
C11 C 0.0649(6) 0.9632(5) 0.13094(17) 0.0273(15) Uani 1 1 d . . .
H17 H 0.1021 0.9780 0.1580 0.033 Uiso 1 1 calc R . .
C13 C 0.1460(7) 1.0094(6) 0.0966(2) 0.0369(17) Uani 1 1 d . . .
H18A H 0.1201 1.0997 0.0889 0.044 Uiso 1 1 calc R . .
H18B H 0.2323 1.0147 0.1063 0.044 Uiso 1 1 calc R . .
C12 C 0.1435(10) 0.9278(9) 0.0613(2) 0.079(4) Uani 1 1 d . . .
H19A H 0.2295 0.9021 0.0547 0.094 Uiso 1 1 calc R . .
H19B H 0.1119 0.9813 0.0387 0.094 Uiso 1 1 calc R . .
C14 C 0.0657(6) 0.8029(6) 0.06440(18) 0.0290(15) Uani 1 1 d . . .
H20 H 0.1031 0.7246 0.0507 0.035 Uiso 1 1 calc R . .
N99 N 0.5000 0.4252(10) 0.2479(3) 0.049(2) Uani 1 2 d S . .
C98 C 0.5000 0.2075(10) 0.2894(3) 0.033(2) Uani 1 2 d S . .
H98A H 0.4726 0.2304 0.3165 0.050 Uiso 0.50 1 calc PR . .
H98B H 0.5838 0.1708 0.2905 0.050 Uiso 0.50 1 calc PR . .
H98C H 0.4436 0.1418 0.2779 0.050 Uiso 0.50 1 calc PR . .
C99 C 0.5000 0.3259(12) 0.2643(3) 0.034(2) Uani 1 2 d S . .
H1 H 0.0000 0.263(7) 0.334(2) 0.011(19) Uiso 1 2 d S . .
H11 H 0.0000 0.421(13) 0.205(4) 0.10(5) Uiso 1 2 d S . .
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'
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
C4 Rh1 C4 40.4(4) . 4 ?
C4 Rh1 N5 90.9(2) . . ?
C4 Rh1 N5 90.9(2) 4 . ?
C4 Rh1 C1 79.6(2) . . ?
C4 Rh1 C1 92.3(2) 4 . ?
N5 Rh1 C1 161.04(16) . . ?
C4 Rh1 C1 92.3(2) . 4 ?
C4 Rh1 C1 79.6(2) 4 4 ?
N5 Rh1 C1 161.05(16) . 4 ?
C1 Rh1 C1 37.3(3) . 4 ?
C4 Rh1 N1 118.6(2) . . ?
C4 Rh1 N1 158.4(2) 4 . ?
N5 Rh1 N1 83.71(17) . . ?
C1 Rh1 N1 86.46(19) . . ?
C1 Rh1 N1 110.9(2) 4 . ?
C4 Rh1 N1 158.4(2) . 4 ?
C4 Rh1 N1 118.6(2) 4 4 ?
N5 Rh1 N1 83.71(17) . 4 ?
C1 Rh1 N1 110.9(2) . 4 ?
C1 Rh1 N1 86.46(19) 4 4 ?
N1 Rh1 N1 81.7(2) . 4 ?
N2 B1 N2 109.9(7) . 4 ?
N2 B1 N6 108.6(5) . . ?
N2 B1 N6 108.6(5) 4 . ?
C8 N5 N6 107.0(7) . . ?
C8 N5 Rh1 132.8(6) . . ?
N6 N5 Rh1 120.2(5) . . ?
C10 N6 N5 108.7(7) . . ?
C10 N6 B1 130.0(7) . . ?
N5 N6 B1 121.3(6) . . ?
C5 N1 N2 106.1(5) . . ?
C5 N1 Rh1 134.5(4) . . ?
N2 N1 Rh1 119.4(3) . . ?
C7 N2 N1 110.2(5) . . ?
C7 N2 B1 130.1(5) . . ?
N1 N2 B1 119.7(5) . . ?
N6 C10 C9 110.0(9) . . ?
C10 C9 C8 103.6(9) . . ?
N5 C8 C9 110.7(9) . . ?
N2 C7 C6 107.9(5) . . ?
C7 C6 C5 104.5(5) . . ?
N1 C5 C6 111.3(5) . . ?
C1 C1 C3 126.2(4) 4 . ?
C1 C1 Rh1 71.37(15) 4 . ?
C3 C1 Rh1 112.8(4) . . ?
C2 C3 C1 115.2(6) . . ?
C3 C2 C4 113.2(7) . . ?
C4 C4 C2 124.8(6) 4 . ?
C4 C4 Rh1 69.82(19) 4 . ?
C2 C4 Rh1 116.5(5) . . ?
C14 Rh11 C14 40.2(4) 4 . ?
C14 Rh11 N15 90.7(2) 4 . ?
C14 Rh11 N15 90.7(2) . . ?
C14 Rh11 C11 80.9(2) 4 4 ?
C14 Rh11 C11 93.7(2) . 4 ?
N15 Rh11 C11 160.96(17) . 4 ?
C14 Rh11 C11 93.7(2) 4 . ?
C14 Rh11 C11 80.9(2) . . ?
N15 Rh11 C11 160.97(17) . . ?
C11 Rh11 C11 37.8(3) 4 . ?
C14 Rh11 N11 158.5(2) 4 . ?
C14 Rh11 N11 118.8(2) . . ?
N15 Rh11 N11 83.66(18) . . ?
C11 Rh11 N11 110.1(2) 4 . ?
C11 Rh11 N11 85.5(2) . . ?
C14 Rh11 N11 118.8(2) 4 4 ?
C14 Rh11 N11 158.5(2) . 4 ?
N15 Rh11 N11 83.66(18) . 4 ?
C11 Rh11 N11 85.5(2) 4 4 ?
C11 Rh11 N11 110.1(2) . 4 ?
N11 Rh11 N11 81.3(2) . 4 ?
N12 B11 N12 108.6(7) . 4 ?
N12 B11 N16 108.4(5) . . ?
N12 B11 N16 108.4(5) 4 . ?
N16 N15 C18 106.2(8) . . ?
N16 N15 Rh11 120.8(5) . . ?
C18 N15 Rh11 133.0(7) . . ?
N15 N16 C20 109.9(7) . . ?
N15 N16 B11 122.6(6) . . ?
C20 N16 B11 127.5(7) . . ?
C15 N11 N12 105.7(5) . . ?
C15 N11 Rh11 134.8(4) . . ?
N12 N11 Rh11 119.3(3) . . ?
C17 N12 N11 109.6(5) . . ?
C17 N12 B11 130.3(6) . . ?
N11 N12 B11 119.9(5) . . ?
N16 C20 C19 105.9(8) . . ?
C18 C19 C20 107.9(9) . . ?
C19 C18 N15 110.1(10) . . ?
N12 C17 C16 108.6(5) . . ?
C17 C16 C15 104.9(6) . . ?
N11 C15 C16 111.2(6) . . ?
C11 C11 C13 125.3(4) 4 . ?
C11 C11 Rh11 71.10(17) 4 . ?
C13 C11 Rh11 111.4(4) . . ?
C12 C13 C11 115.4(6) . . ?
C13 C12 C14 115.6(6) . . ?
C14 C14 C12 123.5(6) 4 . ?
C14 C14 Rh11 69.89(19) 4 . ?
C12 C14 Rh11 114.4(4) . . ?
N99 C99 C98 173.5(13) . . ?
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 C4 2.064(6) . ?
Rh1 C4 2.065(6) 4 ?
Rh1 N5 2.114(7) . ?
Rh1 C1 2.147(5) . ?
Rh1 C1 2.147(5) 4 ?
Rh1 N1 2.251(5) . ?
Rh1 N1 2.251(5) 4 ?
B1 N2 1.523(7) . ?
B1 N2 1.523(7) 4 ?
B1 N6 1.554(12) . ?
N5 C8 1.319(11) . ?
N5 N6 1.378(9) . ?
N6 C10 1.342(12) . ?
N1 C5 1.325(7) . ?
N1 N2 1.364(6) . ?
N2 C7 1.353(7) . ?
C10 C9 1.373(15) . ?
C9 C8 1.417(13) . ?
C7 C6 1.381(9) . ?
C6 C5 1.398(8) . ?
C1 C1 1.372(12) 4 ?
C1 C3 1.498(9) . ?
C3 C2 1.467(10) . ?
C2 C4 1.505(10) . ?
C4 C4 1.425(14) 4 ?
Rh11 C14 2.066(6) 4 ?
Rh11 C14 2.066(6) . ?
Rh11 N15 2.093(7) . ?
Rh11 C11 2.165(6) 4 ?
Rh11 C11 2.165(6) . ?
Rh11 N11 2.245(5) . ?
Rh11 N11 2.245(5) 4 ?
B11 N12 1.528(7) . ?
B11 N12 1.528(7) 4 ?
B11 N16 1.534(12) . ?
N15 N16 1.349(9) . ?
N15 C18 1.350(12) . ?
N16 C20 1.365(11) . ?
N11 C15 1.339(8) . ?
N11 N12 1.366(6) . ?
N12 C17 1.350(7) . ?
C20 C19 1.374(14) . ?
C19 C18 1.334(14) . ?
C17 C16 1.368(9) . ?
C16 C15 1.382(9) . ?
C11 C11 1.403(13) 4 ?
C11 C13 1.517(9) . ?
C13 C12 1.435(10) . ?
C12 C14 1.523(9) . ?
C14 C14 1.421(13) 4 ?
N99 C99 1.144(13) . ?
C98 C99 1.462(15) . ?
