#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:37:07 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301831 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/27/4082751.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_4082751
loop_
_publ_author_name
'Whited, Matthew T.'
'Kosanovich, Alex J.'
'Janzen, Daron E.'
_publ_section_title
;
 Synthesis and Reactivity of Three-Coordinate (dtbpe)Rh Silylamides:
 CO2Bond Cleavage by a Rhodium(I) Disilylamide
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1416
_journal_paper_doi               10.1021/om401130q
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H58 N P2 Rh Si2'
_chemical_formula_sum            'C24 H58 N P2 Rh Si2'
_chemical_formula_weight         581.74
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      52
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.456(4)
_cell_length_b                   17.299(3)
_cell_length_c                   9.0187(17)
_cell_measurement_reflns_used    19247
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.01
_cell_volume                     3191.4(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13'
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26096
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0276P)²+2.2492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2710
_reflns_number_total             3268
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om401130q_si_002.cif
_cod_data_source_block           scu1320_compound2a
_cod_original_cell_volume        3191.4(11)
_cod_database_code               4082751
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, -y, z'
'-x, -y, -z'
'x, -y-1/2, -z-1/2'
'-x-1/2, y-1/2, -z-1/2'
'x-1/2, y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Rh1 Rh 0.03162(2) 0.2500 0.7500 0.02188(9) Uani 1 2 d S T P
P1 P 0.11086(3) 0.16667(4) 0.71376(6) 0.02459(14) Uani 1 1 d . . .
Si1 Si -0.11031(4) 0.26356(4) 0.58624(9) 0.03613(18) Uani 1 1 d . . .
N1 N -0.06834(13) 0.2500 0.7500 0.0286(6) Uani 1 2 d S T P
C1 C -0.13992(15) 0.16941(18) 0.5063(4) 0.0527(8) Uani 1 1 d . . .
H1A H -0.1726 0.1466 0.5727 0.063 Uiso 1 1 calc R U .
H1B H -0.1030 0.1338 0.4956 0.063 Uiso 1 1 calc R U .
H1C H -0.1596 0.1788 0.4089 0.063 Uiso 1 1 calc R U .
C2 C -0.06193(15) 0.31120(18) 0.4362(3) 0.0498(8) Uani 1 1 d . . .
H2A H -0.0234 0.2797 0.4133 0.060 Uiso 1 1 calc R U .
H2B H -0.0479 0.3625 0.4694 0.060 Uiso 1 1 calc R U .
H2C H -0.0891 0.3164 0.3472 0.060 Uiso 1 1 calc R U .
C3 C -0.18371(14) 0.32887(18) 0.6089(4) 0.0549(8) Uani 1 1 d . . .
H3A H -0.1696 0.3789 0.6484 0.066 Uiso 1 1 calc R U .
H3B H -0.2148 0.3051 0.6777 0.066 Uiso 1 1 calc R U .
H3C H -0.2048 0.3365 0.5124 0.066 Uiso 1 1 calc R U .
C4 C 0.11746(13) 0.13235(15) 0.5132(3) 0.0341(6) Uani 1 1 d . . .
C5 C 0.16220(16) 0.06283(18) 0.4854(3) 0.0554(8) Uani 1 1 d . . .
H5A H 0.2046 0.0718 0.5329 0.066 Uiso 1 1 calc R U .
H5B H 0.1685 0.0561 0.3784 0.066 Uiso 1 1 calc R U .
H5C H 0.1421 0.0162 0.5270 0.066 Uiso 1 1 calc R U .
C6 C 0.14484(16) 0.20015(17) 0.4230(3) 0.0490(8) Uani 1 1 d . . .
H6A H 0.1168 0.2455 0.4364 0.059 Uiso 1 1 calc R U .
H6B H 0.1461 0.1861 0.3177 0.059 Uiso 1 1 calc R U .
H6C H 0.1892 0.2122 0.4571 0.059 Uiso 1 1 calc R U .
C7 C 0.04882(16) 0.11507(19) 0.4536(3) 0.0521(8) Uani 1 1 d . . .
H7A H 0.0512 0.1057 0.3465 0.063 Uiso 1 1 calc R U .
H7B H 0.0202 0.1593 0.4728 0.063 Uiso 1 1 calc R U .
H7C H 0.0313 0.0691 0.5031 0.063 Uiso 1 1 calc R U .
C8 C 0.10570(13) 0.07730(14) 0.8361(3) 0.0325(6) Uani 1 1 d . . .
C9 C 0.04400(14) 0.03199(17) 0.7961(3) 0.0448(7) Uani 1 1 d . . .
H9A H 0.0500 0.0068 0.6997 0.054 Uiso 1 1 calc R U .
H9B H 0.0067 0.0674 0.7908 0.054 Uiso 1 1 calc R U .
H9C H 0.0357 -0.0073 0.8720 0.054 Uiso 1 1 calc R U .
C10 C 0.16619(14) 0.02419(17) 0.8308(3) 0.0477(8) Uani 1 1 d . . .
H10A H 0.1669 -0.0037 0.7363 0.057 Uiso 1 1 calc R U .
H10B H 0.1642 -0.0129 0.9128 0.057 Uiso 1 1 calc R U .
H10C H 0.2059 0.0555 0.8400 0.057 Uiso 1 1 calc R U .
C11 C 0.10004(14) 0.10482(15) 0.9977(3) 0.0393(6) Uani 1 1 d . . .
H11A H 0.1414 0.1284 1.0286 0.047 Uiso 1 1 calc R U .
H11B H 0.0902 0.0606 1.0619 0.047 Uiso 1 1 calc R U .
H11C H 0.0649 0.1431 1.0056 0.047 Uiso 1 1 calc R U .
C12 C 0.19343(11) 0.20584(14) 0.7575(3) 0.0312(5) Uani 1 1 d . . .
H12A H 0.2057 0.1913 0.8600 0.037 Uiso 1 1 calc R U .
H12B H 0.2261 0.1833 0.6889 0.037 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 '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'
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'
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
P1 Rh1 P1 84.72(4) . 6_567
N1 Rh1 P1 137.641(18) . .
N1 Rh1 P1 137.642(18) . 6_567
C4 P1 Rh1 113.45(9) . .
C8 P1 Rh1 113.99(8) . .
C8 P1 C4 107.50(11) . .
C12 P1 Rh1 113.55(8) . .
C12 P1 C4 104.48(12) . .
C12 P1 C8 102.89(12) . .
N1 Si1 C1 111.77(11) . .
N1 Si1 C2 114.62(12) . .
N1 Si1 C3 112.59(12) . .
C1 Si1 C3 107.65(14) . .
C2 Si1 C1 105.95(15) . .
C2 Si1 C3 103.62(15) . .
Si1 N1 Rh1 119.86(8) 6_567 .
Si1 N1 Rh1 119.86(8) . .
Si1 N1 Si1 120.28(16) . 6_567
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 P1 116.24(19) . .
C5 C4 C6 107.2(2) . .
C5 C4 C7 109.7(2) . .
C6 C4 P1 106.92(17) . .
C7 C4 P1 109.18(18) . .
C7 C4 C6 107.3(2) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 P1 108.99(17) . .
C9 C8 C10 110.5(2) . .
C9 C8 C11 108.7(2) . .
C10 C8 P1 114.94(18) . .
C11 C8 P1 107.59(17) . .
C11 C8 C10 105.9(2) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
P1 C12 H12A 109.6 . .
P1 C12 H12B 109.6 . .
C12 C12 P1 110.10(10) 6_567 .
C12 C12 H12A 109.6 6_567 .
C12 C12 H12B 109.6 6_567 .
H12A C12 H12B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 P1 2.1937(7) 6_567
Rh1 P1 2.1937(7) .
Rh1 N1 2.045(3) .
P1 C4 1.908(2) .
P1 C8 1.902(2) .
P1 C12 1.862(2) .
Si1 N1 1.7243(15) .
Si1 C1 1.881(3) .
Si1 C2 1.868(3) .
Si1 C3 1.890(3) .
N1 Si1 1.7243(15) 6_567
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.532(4) .
C4 C6 1.534(4) .
C4 C7 1.533(4) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.529(4) .
C8 C10 1.542(3) .
C8 C11 1.537(4) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C12 1.534(5) 6_567
C12 H12A 0.9900 .
C12 H12B 0.9900 .
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_4
Rh1 P1 C12 C12 -25.3(3) 6_567
C1 Si1 N1 Rh1 99.81(12) .
C1 Si1 N1 Si1 -80.19(12) 6_567
C2 Si1 N1 Rh1 -20.75(13) .
C2 Si1 N1 Si1 159.25(13) 6_567
C3 Si1 N1 Rh1 -138.87(11) .
C3 Si1 N1 Si1 41.13(11) 6_567
C4 P1 C12 C12 98.9(2) 6_567
C8 P1 C12 C12 -148.9(2) 6_567
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168332330
