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_4086878
_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         'C30 H20 B F15 N O3 P'
_chemical_formula_sum            'C30 H20 B F15 N O3 P'
_chemical_formula_weight         769.25
_chemical_name_systematic
k1-O-[diethyl-N-(2,6-dimethylphenyl)-O-(tris(pentafluorophenylborane))phosphoramide
_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   mixed
_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                84.979(3)
_cell_angle_beta                 85.688(3)
_cell_angle_gamma                83.649(3)
_cell_formula_units_Z            8
_cell_length_a                   9.7691(10)
_cell_length_b                   21.884(2)
_cell_length_c                   28.934(3)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      2.25
_cell_volume                     6110.7(11)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            135723
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.208
_diffrn_reflns_theta_min         1.221
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.9325
_exptl_absorpt_correction_T_min  0.8440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0497 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.8887.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       prism
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1869
_refine_ls_number_reflns         36105
_refine_ls_number_restraints     1656
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+3.5307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26136
_reflns_number_total             36105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_23
_cod_database_code               4086878
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. 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
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C69(H69A,H69B), C71(H71A,H71B), C39(H39A,H39B),
 C41(H41A,H41B), C99(H99A,H99B), C101(H10G,H10H)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C63(H63), C64(H64), C65(H65), C33(H33), C34(H34),
 C35(H35), C93(H93), C94(H94), C95(H95)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,
 H72C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C100(H10D,H10E,H10F),
 C102(H10I,H10J,H10K)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'