Modulating the Elementary Steps of Methanol Carbonylation by Bridging the Primary and Secondary Coordination Spheres
Gregor, Lauren C.; Grajeda, Javier; Kita, Matthew R.; White, Peter S.; Vetter, Andrew J.; Miller, Alexander J. M.; Organometallics 35 (2016) 3074–; doi:10.1021/acs.organomet.6b00607

data_4088985
_publ_section_title
;
 Modulating the Elementary Steps of Methanol Carbonylation by Bridging the
 Primary and Secondary Coordination Spheres
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3074
_journal_paper_doi               10.1021/acs.organomet.6b00607
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C26 H42 Ir N O7 P, C32 H12 B F24'
_chemical_formula_sum            'C58 H54 B F24 Ir N O7 P'
_chemical_formula_weight         1567.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2346(7)
_cell_length_b                   17.6765(6)
_cell_length_c                   37.7548(14)
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.81
_cell_measurement_theta_min      2.34
_cell_volume                     12169.3(8)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1193
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            104973
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.869
_diffrn_reflns_theta_max         66.869
_diffrn_reflns_theta_min         2.340
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.642
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.6431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0903 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.7170.
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    1.711
_exptl_crystal_description       plate
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         10776
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0342P)^2^+44.6698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7840
_reflns_number_total             10776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00607_si_002.cif
_cod_data_source_block           x1511007
_cod_database_code               4088985
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.483
_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
 C90, F91, F92, F93, F94, F95, F96
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(F94)=Sof(F95)=Sof(F96)=1-FVAR(1)
 Sof(F91)=Sof(F92)=Sof(F93)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,
 H27B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B),
 C35(H35A,H35B), C36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C39(H39), C41(H41), C43(H43), C53(H53),
 C55(H55), C57(H57), C67(H67), C69(H69), C71(H71), C81(H81), C83(H83), C85(H85)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              16261
_shelx_hkl_checksum              91989
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'