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_4086869
_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         'C28 H46 B N O3 P Rh'
_chemical_formula_sum            'C28 H46 B N O3 P Rh'
_chemical_formula_weight         589.35
_chemical_name_systematic
n4-cyclooctadiene-k2-N,H-[diethyl-N-(2,6-dimethylphenyl)-O-(9-borabicyclononane)phosphoramidato]rhodium(I)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-28
_audit_creation_method
;
Olex2 1.2
(compiled Sep  9 2016 15:39:09 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                105.020(4)
_cell_angle_beta                 104.542(3)
_cell_angle_gamma                100.693(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3803(19)
_cell_length_b                   10.4864(19)
_cell_length_c                   14.300(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.296
_cell_measurement_theta_min      2.535
_cell_volume                     1402.0(5)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20341
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.364
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9264
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0535 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.8097.
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    1.396
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.322
_refine_diff_density_min         -1.622
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0582
_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/[\s^2^(Fo^2^)+(0.0669P)^2^+7.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6372
_reflns_number_total             7506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_5
_cod_original_cell_volume        1402.0(4)
_cod_database_code               4086869
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C21(H21), C25(H25), B1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C17(H17A,H17B), C19(H19A,
 H19B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'