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_4088984
_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 H41 Ir N O7 P'
_chemical_formula_sum            'C25 H41 Ir N O7 P'
_chemical_formula_weight         690.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.644(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.127(2)
_cell_length_b                   7.9807(11)
_cell_length_c                   19.276(3)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.00
_cell_measurement_theta_min      3.03
_cell_volume                     2721.0(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.308
_diffrn_reflns_theta_min         3.032
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.416
_exptl_absorpt_correction_T_max  0.5645
_exptl_absorpt_correction_T_min  0.2234
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.3957.
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    1.686
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.071
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0237P)^2^+8.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5017
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00607_si_002.cif
_cod_data_source_block           x1604007
_cod_database_code               4088984
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.195
_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.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,
 H26B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B),
 C34(H34A,H34B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              56827
_shelx_hkl_checksum              61776
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-25
_olex2_date_sample_submission    2016-04-25
_olex2_submission_original_sample_id (MeO-15c5)Ir(CO)
_olex2_submission_special_instructions 'No special instructions were received'