Accessing δ-B‒H Coordinated Complexes of Rh(I) and Ir(I) Using Mono- and Dihydroboranes: Cooperative Stabilization by a Phosphoramidate Coligand
Drover, Marcus W.; Bowes, Eric G.; Love, Jennifer A.; Schafer, Laurel L.; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00784

data_4086877
_publ_section_title
;
 Accessing \d-B--H Coordinated Complexes of Rh(I) and Ir(I) Using Mono-
 and Dihydroboranes: Cooperative Stabilization by a Phosphoramidate
 Coligand
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00784
_journal_year                    2016
_chemical_formula_moiety         'C38 H31 B F15 N O3 P Rh'
_chemical_formula_sum            'C38 H31 B F15 N O3 P Rh'
_chemical_formula_weight         979.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-29
_audit_creation_method
;
Olex2 1.2
(compiled Sep  9 2016 15:39:09 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.230(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.307(3)
_cell_length_b                   16.551(4)
_cell_length_c                   22.006(5)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    90
_cell_measurement_theta_max      22.613
_cell_measurement_theta_min      2.457
_cell_volume                     3743.8(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.476
_diffrn_reflns_theta_min         1.230
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.7741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0906 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.8283. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.945
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         10188
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0722
_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/[\s^2^(Fo^2^)+(0.0831P)^2^+45.1726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8758
_reflns_number_total             10188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_21
_cod_original_cell_volume        3743.6(16)
_cod_database_code               4086877
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7753(14) 0.2247(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C5(H5), C1(H1), C2(H2), C6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C7(H7A,H7B), C4(H4A,H4B), C3(H3A,H3B), C17(H17A,H17B), C8(H8A,
 H8B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C18(H18A,H18B,
 H18C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'