#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:45:10 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178699 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/10/4081036.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_4081036
loop_
_publ_author_name
'Pettinari, Riccardo'
'Pettinari, Claudio'
'Marchetti, Fabio'
'Monari, Magda'
'Mosconi, Edoardo'
'De Angelis, Filippo'
_publ_section_title
;
 Boron Functionalization and Unusual B--C Bond Activation in Rhodium(III)
 and Iridium(III) Complexes with Diphenylbis(pyrazolylborate) Ligands
 (Ph2Bp)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3895
_journal_paper_doi               10.1021/om400375j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C28 H31 B Cl N4 O Rh'
_chemical_formula_weight         588.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   23.699(3)
_cell_length_b                   10.6026(13)
_cell_length_c                   11.8624(15)
_cell_measurement_reflns_used    2486
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.18
_cell_measurement_theta_min      2.43
_cell_volume                     2980.7(6)
_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  'Bruker SHELXTL'
_computing_structure_solution    'SIR-97, Giacovazzo 1999'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24308
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3727
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0530
_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)+(0.0961P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                1920
_reflns_number_total             3727
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om400375j_si_007.cif
_cod_data_source_block           comp-1
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4081036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
Rh Rh 0.90258(2) 0.2500 0.93555(5) 0.0618(2) Uani 1 2 d S . .
Cl Cl 0.99500(8) 0.2500 1.02291(19) 0.0839(6) Uani 1 2 d S . .
N1 N 0.87927(17) 0.3845(4) 1.0552(3) 0.0606(10) Uani 1 1 d . . .
N2 N 0.84198(16) 0.3684(3) 1.1409(3) 0.0613(10) Uani 1 1 d . . .
C1 C 0.9001(2) 0.5005(5) 1.0646(5) 0.0835(17) Uani 1 1 d . . .
H1 H 0.9270 0.5354 1.0168 0.100 Uiso 1 1 calc R . .
C3 C 0.8405(3) 0.4764(5) 1.2015(5) 0.0831(16) Uani 1 1 d . . .
H3 H 0.8184 0.4903 1.2652 0.100 Uiso 1 1 calc R . .
C2 C 0.8762(3) 0.5612(5) 1.1546(6) 0.0918(18) Uani 1 1 d . . .
H2 H 0.8831 0.6433 1.1785 0.110 Uiso 1 1 calc R . .
C4 C 0.7858(4) 0.2500 1.2946(6) 0.074(2) Uani 1 2 d S . .
C5 C 0.8254(5) 0.2500 1.3790(7) 0.102(3) Uani 1 2 d S . .
H5 H 0.8634 0.2500 1.3599 0.123 Uiso 1 2 calc SR . .
C6 C 0.8103(6) 0.2500 1.4918(9) 0.120(4) Uani 1 2 d S . .
H6 H 0.8379 0.2500 1.5474 0.144 Uiso 1 2 calc SR . .
C7 C 0.7560(7) 0.2500 1.5202(9) 0.133(5) Uani 1 2 d S . .
H7 H 0.7464 0.2500 1.5962 0.159 Uiso 1 2 calc SR . .
C8 C 0.7133(6) 0.2500 1.4402(8) 0.114(4) Uani 1 2 d S . .
H8 H 0.6754 0.2500 1.4606 0.137 Uiso 1 2 calc SR . .
C9 C 0.7302(4) 0.2500 1.3286(6) 0.085(2) Uani 1 2 d S . .
H9 H 0.7024 0.2500 1.2732 0.102 Uiso 1 2 calc SR . .
C10 C 0.7493(3) 0.2500 1.0806(5) 0.0596(17) Uani 1 2 d S . .
C11 C 0.7224(2) 0.3604(6) 1.0498(4) 0.0804(15) Uani 1 1 d . . .
H11 H 0.7394 0.4369 1.0679 0.096 Uiso 1 1 calc R . .
C12 C 0.6718(3) 0.3618(7) 0.9938(5) 0.104(2) Uani 1 1 d . . .
H12 H 0.6551 0.4382 0.9749 0.125 Uiso 1 1 calc R . .
C13 C 0.6456(4) 0.2500 0.9654(8) 0.120(4) Uani 1 2 d S . .
H13 H 0.6111 0.2500 0.9280 0.144 Uiso 1 2 calc SR . .
C14 C 0.9390(4) 0.2500 0.7680(9) 0.147(6) Uani 1 2 d SDU . .
C15 C 0.9058(3) 0.3590(7) 0.7821(5) 0.112(3) Uani 1 1 d DU . .
C16 C 0.8509(2) 0.3159(4) 0.7990(4) 0.0695(13) Uani 1 1 d DU . .
B B 0.8048(4) 0.2500 1.1613(7) 0.066(2) Uani 1 2 d S . .
C19 C 0.8005(3) 0.3993(8) 0.8081(5) 0.145(3) Uani 1 1 d DU . .
H19A H 0.8074 0.4635 0.8634 0.217 Uiso 1 1 calc R . .
H19B H 0.7683 0.3501 0.8304 0.217 Uiso 1 1 calc R . .
H19C H 0.7932 0.4379 0.7364 0.217 Uiso 1 1 calc R . .
C18 C 0.9235(6) 0.4952(10) 0.7719(8) 0.256(8) Uani 1 1 d DU . .
H18A H 0.9614 0.5047 0.7991 0.383 Uiso 1 1 calc R . .
H18B H 0.8986 0.5470 0.8159 0.383 Uiso 1 1 calc R . .
H18C H 0.9217 0.5206 0.6943 0.383 Uiso 1 1 calc R . .
C17 C 1.0014(4) 0.2500 0.7406(11) 0.290(13) Uani 1 2 d SDU . .
H17A H 1.0071 0.2152 0.6668 0.435 Uiso 0.50 1 calc PR A -1
H17B H 1.0213 0.1999 0.7951 0.435 Uiso 0.50 1 calc PR A -1
H17C H 1.0155 0.3349 0.7425 0.435 Uiso 0.50 1 calc PR A -1
O1W O 0.9722(14) 0.2500 1.327(4) 1.06(5) Uani 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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 Rh N1 86.2(2) . 8_565
N1 Rh C16 125.75(16) . 8_565
N1 Rh C16 98.04(16) 8_565 8_565
N1 Rh C16 98.04(16) . .
N1 Rh C16 125.75(16) 8_565 .
C16 Rh C16 38.0(2) 8_565 .
N1 Rh C15 161.69(19) . 8_565
N1 Rh C15 102.6(2) 8_565 8_565
C16 Rh C15 37.77(18) 8_565 8_565
C16 Rh C15 63.8(2) . 8_565
N1 Rh C15 102.6(2) . .
N1 Rh C15 161.69(19) 8_565 .
C16 Rh C15 63.8(2) 8_565 .
C16 Rh C15 37.77(18) . .
C15 Rh C15 64.8(4) 8_565 .
N1 Rh C14 136.85(11) . .
N1 Rh C14 136.85(11) 8_565 .
C16 Rh C14 62.3(3) 8_565 .
C16 Rh C14 62.3(3) . .
C15 Rh C14 38.0(2) 8_565 .
C15 Rh C14 38.0(2) . .
N1 Rh Cl 87.04(11) . .
N1 Rh Cl 87.04(11) 8_565 .
C16 Rh Cl 146.96(14) 8_565 .
C16 Rh Cl 146.96(14) . .
C15 Rh Cl 109.22(18) 8_565 .
C15 Rh Cl 109.22(18) . .
C14 Rh Cl 91.9(3) . .
C1 N1 N2 107.1(4) . .
C1 N1 Rh 126.2(4) . .
N2 N1 Rh 126.6(3) . .
C3 N2 N1 108.0(4) . .
C3 N2 B 125.9(5) . .
N1 N2 B 126.0(4) . .
N1 C1 C2 110.3(5) . .
N1 C1 H1 124.8 . .
C2 C1 H1 124.8 . .
N2 C3 C2 109.1(5) . .
N2 C3 H3 125.5 . .
C2 C3 H3 125.5 . .
C3 C2 C1 105.5(5) . .
C3 C2 H2 127.3 . .
C1 C2 H2 127.3 . .
C5 C4 C9 116.1(8) . .
C5 C4 B 121.0(8) . .
C9 C4 B 122.9(7) . .
C4 C5 C6 121.9(10) . .
C4 C5 H5 119.1 . .
C6 C5 H5 119.0 . .
C7 C6 C5 119.7(11) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.2 . .
C6 C7 C8 122.2(11) . .
C6 C7 H7 118.9 . .
C8 C7 H7 118.9 . .
C9 C8 C7 116.3(12) . .
C9 C8 H8 121.8 . .
C7 C8 H8 121.9 . .
C8 C9 C4 123.9(9) . .
C8 C9 H9 118.1 . .
C4 C9 H9 118.0 . .
C11 C10 C11 115.8(7) 8_565 .
C11 C10 B 121.9(3) 8_565 .
C11 C10 B 121.9(3) . .
C12 C11 C10 122.7(6) . .
C12 C11 H11 118.6 . .
C10 C11 H11 118.7 . .
C13 C12 C11 120.2(7) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C12 C13 C12 118.4(9) . 8_565
C12 C13 H13 120.8 . .
C12 C13 H13 120.8 8_565 .
C15 C14 C15 110.3(8) . 8_565
C15 C14 C17 124.8(4) . .
C15 C14 C17 124.8(4) 8_565 .
C15 C14 Rh 70.7(5) . .
C15 C14 Rh 70.7(5) 8_565 .
C17 C14 Rh 125.9(8) . .
C16 C15 C14 105.7(6) . .
C16 C15 C18 125.8(9) . .
C14 C15 C18 128.4(8) . .
C16 C15 Rh 70.8(3) . .
C14 C15 Rh 71.3(6) . .
C18 C15 Rh 126.1(5) . .
C16 C16 C15 109.1(4) 8_565 .
C16 C16 C19 126.4(4) 8_565 .
C15 C16 C19 124.4(6) . .
C16 C16 Rh 71.02(12) 8_565 .
C15 C16 Rh 71.5(3) . .
C19 C16 Rh 126.5(4) . .
N2 B N2 107.8(6) . 8_565
N2 B C10 111.5(4) . .
N2 B C10 111.5(4) 8_565 .
N2 B C4 107.8(4) . .
N2 B C4 107.8(4) 8_565 .
C10 B C4 110.2(6) . .
C16 C19 H19A 109.5 . .
C16 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C16 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.4 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh N1 2.086(4) .
Rh N1 2.086(4) 8_565
Rh C16 2.148(5) 8_565
Rh C16 2.148(5) .
Rh C15 2.157(6) 8_565
Rh C15 2.157(6) .
Rh C14 2.166(10) .
Rh Cl 2.4231(18) .
N1 C1 1.330(7) .
N1 N2 1.358(5) .
N2 C3 1.353(6) .
N2 B 1.554(6) .
C1 C2 1.369(8) .
C1 H1 0.9300 .
C3 C2 1.354(8) .
C3 H3 0.9300 .
C2 H2 0.9300 .
C4 C5 1.372(11) .
C4 C9 1.379(11) .
C4 B 1.643(11) .
C5 C6 1.386(13) .
C5 H5 0.9300 .
C6 C7 1.328(16) .
C6 H6 0.9300 .
C7 C8 1.388(16) .
C7 H7 0.9300 .
C8 C9 1.384(11) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C11 1.382(6) 8_565
C10 C11 1.382(6) .
C10 B 1.626(10) .
C11 C12 1.372(8) .
C11 H11 0.9300 .
C12 C13 1.379(8) .
C12 H12 0.9300 .
C13 C12 1.379(8) 8_565
C13 H13 0.9300 .
C14 C15 1.408(8) .
C14 C15 1.408(8) 8_565
C14 C17 1.516(12) .
C15 C16 1.394(7) .
C15 C18 1.509(10) .
C16 C16 1.397(9) 8_565
C16 C19 1.490(7) .
B N2 1.554(6) 8_565
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
