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_4086872
_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         'C32 H32 B F10 N O3 P Rh, 0.5(C7 H8)'
_chemical_formula_sum            'C35.5 H36 B F10 N O3 P Rh'
_chemical_formula_weight         859.34
_chemical_name_systematic
n4-cyclooctadiene-k2-N,H-[diethyl-N-(2,6-dimethylphenyl)-O-(bis(pentafluorophenyl)borane)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                73.927(2)
_cell_angle_beta                 79.174(3)
_cell_angle_gamma                87.851(3)
_cell_formula_units_Z            4
_cell_length_a                   9.5021(12)
_cell_length_b                   19.939(3)
_cell_length_c                   19.973(3)
_cell_measurement_reflns_used    9279
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.262
_cell_measurement_theta_min      2.442
_cell_volume                     3571.1(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69840
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.321
_diffrn_reflns_theta_min         1.290
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.8833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0481 before and 0.0373 after correction.
The Ratio of minimum to maximum transmission is 0.9051.
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    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.999
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         19107
_refine_ls_number_restraints     931
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0307P)^2^+18.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16855
_reflns_number_total             19107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00784_si_002.cif
_cod_data_source_block           Complex_11
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C71 H72 B2 F20 N2 O6 P2 Rh2'
_cod_original_formula_weight         1718.68
_cod_original_formula_moiety         '2(C32 H32 B F10 N O3 P Rh), C7 H8'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3571.2(8)
_cod_database_code               4086872
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.810
_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. Restrained planarity
 C65, C66, C67, C68, C69, C70, C71
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.02
4. 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
5.a Free rotating group:
 C65(C66,C67,C68,C69,C70,C71)
5.b Ternary CH refined with riding coordinates:
 C33(H33), C34(H34), C37(H37), C38(H38), B2(H2), C1(H1), C2(H2A), C5(H5),
 C6(H6), B1(H1A)
5.c Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C39(H39A,H39B), C40(H40A,H40B), C49(H49A,
 H49B), C51(H51A,H51B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B),
 C17(H17A,H17B), C19(H19A,H19B)
5.d Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C45(H45), C11(H11), C12(H12), C13(H13), C67(H67),
 C68(H68), C69(H69), C70(H70), C71(H71)
5.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C65(H65A,H65B,H65C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'