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_1549495
_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 H44 Cl Ir N O7 P'
_chemical_formula_sum            'C26 H44 Cl Ir N O7 P'
_chemical_formula_weight         741.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6431(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0632(4)
_cell_length_b                   12.3425(3)
_cell_length_c                   16.2371(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.00
_cell_measurement_theta_min      3.08
_cell_volume                     2876.77(13)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.190
_diffrn_reflns_theta_min         3.078
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.732
_exptl_absorpt_correction_T_max  0.753301
_exptl_absorpt_correction_T_min  0.442147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0729 before and 0.0427 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1508 before and 0.0590 after correction.
 The Ratio of minimum to maximum transmission is 0.59.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 52865 reflections, Rint = 0.0456
 (34591 with I > 3sig(I), Rint = 0.0407)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         51638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0398P)^2^+0.6810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42887
_reflns_number_total             51638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy00328a2.cif
_cod_data_source_block           x1510003
_cod_depositor_comments
'Adding full bibliography for 1549495--1549496.cif.'
_cod_database_code               1549495
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.287
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7005(6) 0.2995(6)
2. 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
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,
 H22B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              13863
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'