Salt-promoted catalytic methanol carbonylation using iridium pincer-crown ether complexes
Gregor, Lauren C.; Grajeda, Javier; White, Peter S.; Vetter, Andrew J.; Miller, Alexander J. M.; Catalysis Science & Technology 8 (2018) 3133–; doi:10.1039/C8CY00328A

data_1549496
_publ_section_title
;
 Salt-promoted catalytic methanol carbonylation using iridium pincer-crown
 ether complexes
;
_journal_issue                   12
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3133
_journal_paper_doi               10.1039/C8CY00328A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C26 H43 Ir N O7 P'
_chemical_formula_sum            'C26 H43 Ir N O7 P'
_chemical_formula_weight         704.78
_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             2015-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                89.185(4)
_cell_angle_beta                 82.743(4)
_cell_angle_gamma                89.582(5)
_cell_formula_units_Z            4
_cell_length_a                   7.7588(6)
_cell_length_b                   15.5942(12)
_cell_length_c                   24.1160(19)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.11
_cell_measurement_theta_min      3.40
_cell_volume                     2894.1(4)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.968
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            114739
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.274
_diffrn_reflns_theta_min         1.847
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.806
_exptl_absorpt_correction_T_max  0.5425
_exptl_absorpt_correction_T_min  0.2436
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0708 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.4490.
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    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         11097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+3.4326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9754
_reflns_number_total             11097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy00328a2.cif
_cod_data_source_block           x1509008
_cod_depositor_comments
'Adding full bibliography for 1549495--1549496.cif.'
_cod_database_code               1549496
_shelx_estimated_absorpt_t_max   0.459
_shelx_estimated_absorpt_t_min   0.246
_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:
 C3(H3), C6(H6), C37(H37), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), 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), C52(H52A,H52B),
  C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C60(H60A,
 H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C66(H66A,H66B),
 C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C47(H47), C48(H48), C49(H49)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              90206
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'