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_4088983
_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         'C25 H42 I Ir N O6 P'
_chemical_formula_sum            'C25 H42 I Ir N O6 P'
_chemical_formula_weight         802.67
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.3658(2)
_cell_length_b                   14.7653(3)
_cell_length_c                   40.8371(9)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      72.24
_cell_measurement_theta_min      5.20
_cell_volume                     5647.3(2)
_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      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            74407
_diffrn_reflns_theta_full        72.46
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         5.20
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.593
_exptl_absorpt_correction_T_max  0.3452
_exptl_absorpt_correction_T_min  0.0850
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1143 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.2462.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.709
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+13.4504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                5410
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00607_si_002.cif
_cod_data_source_block           jg128abscorr
_cod_database_code               4088983
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.022) H11(0.025) H1A(0.033) H1B(0.033) H1C(0.033)
 H24A(0.028) H24B(0.028) H16A(0.025) H16B(0.025) H15A(0.023) H15B(0.023)
 H25A(0.024) H25B(0.024) H12(0.025) H8A(0.048) H8B(0.048) H8C(0.048) H3(0.024)
 H6(0.025) H7A(0.04) H7B(0.04) H7C(0.04) H5A(0.041) H5B(0.041) H5C(0.041)
 H19A(0.028) H19B(0.028) H18A(0.027) H18B(0.027) H17A(0.03) H17B(0.03)
 H20A(0.031) H20B(0.031) H21A(0.031) H21B(0.031) H22A(0.028) H22B(0.028)
 H23A(0.027) H23B(0.027) H4A(0.04) H4B(0.04) H4C(0.04)
 Fixed X: H10(0.0779) H11(-0.1393) H1A(0.23) H1B(0.2532) H1C(0.3449)
 H24A(0.0235) H24B(-0.0107) H16A(0.0166) H16B(0.0647) H15A(-0.2525) H15B(-
 0.2535) H25A(-0.2235) H25B(-0.2117) H12(-0.2627) H8A(0.3991) H8B(0.5609)
 H8C(0.4561) H3(0.0471) H6(0.4364) H7A(0.4956) H7B(0.6103) H7C(0.4817)
 H5A(0.1506) H5B(0.1342) H5C(0.287) H19A(-0.2451) H19B(-0.3167) H18A(-0.1826)
 H18B(-0.3093) H17A(-0.214) H17B(-0.0815) H20A(-0.0439) H20B(-0.2046) H21A(-
 0.0282) H21B(0.0275) H22A(-0.0619) H22B(-0.2091) H23A(-0.0134) H23B(0.042)
 H4A(0.3106) H4B(0.1587) H4C(0.1878)
 Fixed Y: H10(0.2533) H11(0.1775) H1A(0.2622) H1B(0.301) H1C(0.3405)
 H24A(0.3669) H24B(0.4695) H16A(0.2097) H16B(0.2542) H15A(0.2612) H15B(0.3663)
 H25A(0.3338) H25B(0.4287) H12(0.2007) H8A(0.5712) H8B(0.5413) H8C(0.4762)
 H3(0.5373) H6(0.519) H7A(0.3447) H7B(0.4089) H7C(0.3665) H5A(0.6375)
 H5B(0.6837) H5C(0.6483) H19A(0.259) H19B(0.1679) H18A(0.0861) H18B(0.1485)
 H17A(0.1808) H17B(0.114) H20A(0.1837) H20B(0.2164) H21A(0.3354) H21B(0.3199)
 H22A(0.4852) H22B(0.4978) H23A(0.5201) H23B(0.4194) H4A(0.5483) H4B(0.5821)
 H4C(0.4763)
 Fixed Z: H10(0.5011) H11(0.5112) H1A(0.6054) H1B(0.6416) H1C(0.6118)
 H24A(0.6957) H24B(0.6851) H16A(0.629) H16B(0.6628) H15A(0.6188) H15B(0.6091)
 H25A(0.6759) H25B(0.6572) H12(0.5601) H8A(0.6026) H8B(0.5961) H8C(0.6162)
 H3(0.5387) H6(0.5486) H7A(0.5753) H7B(0.5578) H7C(0.537) H5A(0.5773)
 H5B(0.5421) H5C(0.554) H19A(0.75) H19B(0.7638) H18A(0.7217) H18B(0.7079)
 H17A(0.6583) H17B(0.6643) H20A(0.8174) H20B(0.8114) H21A(0.8231) H21B(0.7864)
 H22A(0.7955) H22B(0.7762) H23A(0.7408) H23B(0.7483) H4A(0.5036) H4B(0.4905)
 H4C(0.4956)
;
_olex2_submission_original_sample_id JG128
_olex2_submission_special_instructions 'No special instructions were received'