#------------------------------------------------------------------------------
#$Date: 2015-06-07 01:27:35 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138571 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/48/7034813.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_7034813
loop_
_publ_author_name
'Borner, C.'
'Brandhorst, K.'
'Kleeberg, C.'
_publ_section_title
;
 Selective B-B bond activation in an unsymmetrical diborane(4) by
 [(Me3P)4Rh-X] (X = Me, OtBu): a switch of mechanism?
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8600
_journal_page_last               8604
_journal_paper_doi               10.1039/c5dt00618j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C17 H37 B N2 P3 Rh'
_chemical_formula_sum            'C17 H37 B N2 P3 Rh'
_chemical_formula_weight         476.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-04 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.66500(10)
_cell_length_b                   13.9554(2)
_cell_length_c                   12.2545(2)
_cell_measurement_reflns_used    39289
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      3.31
_cell_volume                     1139.48(3)
_computing_cell_refinement
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 WinGX v2013.2 (L. J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854.)
;
_computing_structure_refinement
;
 SHELXL-2013 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_structure_solution
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_diffrn_ambient_temperature      102(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            105629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.212
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       'fragment of rhombohedral'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3327
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0334P)²+1.4491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                3136
_reflns_number_total             3327
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt00618j2.cif
_cod_data_source_block           cb33ck
_cod_depositor_comments
'Adding full bibliography for 7034812--7034816.cif.'
_cod_database_code               7034813
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.6591(3) -0.04308(12) 0.27822(14) 0.0163(3) Uani 1 1 d . . .
C2 C 0.5664(3) -0.12858(13) 0.30589(15) 0.0203(3) Uani 1 1 d . . .
H2 H 0.4434 -0.1288 0.3435 0.024 Uiso 1 1 calc R U .
C3 C 0.6596(3) -0.21442(13) 0.27678(15) 0.0228(4) Uani 1 1 d . . .
H3 H 0.5979 -0.2737 0.2940 0.027 Uiso 1 1 calc R U .
C4 C 0.4299(3) 0.07498(14) 0.35907(17) 0.0248(4) Uani 1 1 d . . .
H4A H 0.3164 0.0345 0.3362 0.037 Uiso 1 1 calc R U .
H4B H 0.3949 0.1425 0.3474 0.037 Uiso 1 1 calc R U .
H4C H 0.4612 0.0642 0.4367 0.037 Uiso 1 1 calc R U .
C5 C 0.7434(4) 0.29994(15) -0.03322(16) 0.0285(4) Uani 1 1 d . . .
H5A H 0.8774 0.2713 -0.0365 0.043 Uiso 1 1 calc R U .
H5B H 0.7561 0.3693 -0.0224 0.043 Uiso 1 1 calc R U .
H5C H 0.6692 0.2873 -0.1017 0.043 Uiso 1 1 calc R U .
C6 C 0.3583(3) 0.30031(15) 0.06185(18) 0.0286(4) Uani 1 1 d . . .
H6A H 0.3020 0.2815 -0.0096 0.043 Uiso 1 1 calc R U .
H6B H 0.3688 0.3703 0.0655 0.043 Uiso 1 1 calc R U .
H6C H 0.2705 0.2775 0.1194 0.043 Uiso 1 1 calc R U .
C7 C 0.5596(3) 0.12887(13) 0.02161(16) 0.0237(4) Uani 1 1 d . . .
H7A H 0.4752 0.0917 0.0704 0.036 Uiso 1 1 calc R U .
H7B H 0.6873 0.0954 0.0121 0.036 Uiso 1 1 calc R U .
H7C H 0.4906 0.1362 -0.0494 0.036 Uiso 1 1 calc R U .
C8 C 0.9900(5) 0.4697(3) 0.1953(4) 0.0537(15) Uani 0.5 1 d D . P
H8A H 1.0085 0.5384 0.2086 0.080 Uiso 0.5 1 calc R U P
H8B H 0.9906 0.4572 0.1166 0.080 Uiso 0.5 1 calc R U P
H8C H 1.0994 0.4339 0.2314 0.080 Uiso 0.5 1 calc R U P
C9 C 0.5905(7) 0.5073(3) 0.1630(3) 0.0378(11) Uani 0.5 1 d D . P
H9A H 0.4513 0.5028 0.1866 0.057 Uiso 0.5 1 calc R U P
H9B H 0.5984 0.4859 0.0871 0.057 Uiso 0.5 1 calc R U P
H9C H 0.6361 0.5739 0.1688 0.057 Uiso 0.5 1 calc R U P
C10 C 0.7555(6) 0.5087(3) 0.3700(3) 0.0355(10) Uani 0.5 1 d D . P
H10A H 0.7825 0.5748 0.3477 0.053 Uiso 0.5 1 calc R U P
H10B H 0.8615 0.4871 0.4211 0.053 Uiso 0.5 1 calc R U P
H10C H 0.6256 0.5058 0.4056 0.053 Uiso 0.5 1 calc R U P
B1 B 0.7500 0.11649(19) 0.2500 0.0166(5) Uani 1 2 d S T P
N1 N 0.6030(2) 0.05109(11) 0.29558(12) 0.0180(3) Uani 1 1 d . . .
P1 P 0.60782(8) 0.24736(3) 0.08102(4) 0.01874(10) Uani 1 1 d . . .
P2 P 0.7500 0.43131(5) 0.2500 0.02746(16) Uani 1 2 d DS T P
Rh1 Rh 0.7500 0.26511(2) 0.2500 0.01679(7) Uani 1 2 d S T P
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'
P P 0.1023 0.0942 '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 C1 C2 130.90(16) . .
N1 C1 C1 108.29(9) . 2_655
C2 C1 C1 120.81(10) . 2_655
C1 C2 C3 118.05(17) . .
C3 C3 C2 121.13(11) 2_655 .
N1 B1 N1 102.6(2) 2_655 .
N1 B1 Rh1 128.69(10) 2_655 .
N1 B1 Rh1 128.69(10) . .
C1 N1 C4 121.56(15) . .
C1 N1 B1 110.40(15) . .
C4 N1 B1 127.83(15) . .
C6 P1 C7 99.42(10) . .
C6 P1 C5 101.74(11) . .
C7 P1 C5 98.19(9) . .
C6 P1 Rh1 115.52(7) . .
C7 P1 Rh1 121.76(7) . .
C5 P1 Rh1 116.69(7) . .
C10 P2 C10 107.4(3) . 2_655
C10 P2 C9 35.49(18) . 2_655
C10 P2 C9 97.28(13) 2_655 2_655
C10 P2 C9 97.28(13) . .
C10 P2 C9 35.49(18) 2_655 .
C9 P2 C9 109.0(3) 2_655 .
C10 P2 C8 96.97(13) . .
C10 P2 C8 62.11(16) 2_655 .
C9 P2 C8 62.75(15) 2_655 .
C9 P2 C8 96.79(13) . .
C10 P2 C8 62.11(16) . 2_655
C10 P2 C8 96.97(13) 2_655 2_655
C9 P2 C8 96.79(13) 2_655 2_655
C9 P2 C8 62.75(15) . 2_655
C8 P2 C8 146.0(3) . 2_655
C10 P2 Rh1 126.31(14) . .
C10 P2 Rh1 126.31(14) 2_655 .
C9 P2 Rh1 125.48(14) 2_655 .
C9 P2 Rh1 125.48(14) . .
C8 P2 Rh1 107.01(16) . .
C8 P2 Rh1 107.01(16) 2_655 .
B1 Rh1 P1 83.732(12) . .
B1 Rh1 P1 83.731(12) . 2_655
P1 Rh1 P1 167.46(2) . 2_655
B1 Rh1 P2 180.0 . .
P1 Rh1 P2 96.268(12) . .
P1 Rh1 P2 96.269(12) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.384(2) .
C1 C2 1.389(2) .
C1 C1 1.410(3) 2_655
C2 C3 1.400(3) .
C3 C3 1.386(4) 2_655
C4 N1 1.446(2) .
C5 P1 1.838(2) .
C6 P1 1.830(2) .
C7 P1 1.8318(19) .
C8 P2 1.829(3) .
C9 P2 1.826(3) .
C10 P2 1.824(3) .
B1 N1 1.460(2) 2_655
B1 N1 1.460(2) .
B1 Rh1 2.074(3) .
P1 Rh1 2.2697(5) .
P2 C10 1.824(3) 2_655
P2 C9 1.826(3) 2_655
P2 C8 1.829(3) 2_655
P2 Rh1 2.3194(7) .
Rh1 P1 2.2697(5) 2_655
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
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 179.73(18) . .
C1 C1 C2 C3 0.4(3) 2_655 .
C1 C2 C3 C3 0.9(3) . 2_655
C2 C1 N1 C4 5.4(3) . .
C1 C1 N1 C4 -175.20(18) 2_655 .
C2 C1 N1 B1 -179.39(16) . .
C1 C1 N1 B1 0.0(2) 2_655 .
N1 B1 N1 C1 0.01(9) 2_655 .
Rh1 B1 N1 C1 -179.99(9) . .
N1 B1 N1 C4 174.8(2) 2_655 .
Rh1 B1 N1 C4 -5.2(2) . .
