Electronic effects on the catalytic disproportionation of formic acid to methanol by [Cp*Ir(III)(R-bpy)Cl]Cl complexes.
Sasayama, A. F.; Moore, C. E.; Kubiak, C. P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2436–2439; doi:10.1039/c5dt04606h

data_7037965
_publ_section_title
;
 Electronic effects on the catalytic disproportionation of formic acid to
 methanol by [Cp*Ir(III)(R-bpy)Cl]Cl complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2436
_journal_page_last               2439
_journal_paper_doi               10.1039/c5dt04606h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H21 Cl F6 Ir N2, Cl, 0.5(H2 O)'
_chemical_formula_sum            'C22 H22 Cl2 F6 Ir N2 O0.5'
_chemical_formula_weight         699.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-18 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.000(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2237(5)
_cell_length_b                   15.7371(4)
_cell_length_c                   21.8522(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.453
_cell_measurement_theta_min      2.294
_cell_volume                     5275.2(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.627
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.321
_exptl_absorpt_correction_T_max  0.0452
_exptl_absorpt_correction_T_min  0.0239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.5288.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'Yellow Orange'
_exptl_crystal_colour_modifier   Yellow
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       Block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.067
_refine_diff_density_max         2.159
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         10796
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0277P)^2^+5.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8428
_reflns_number_total             10796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04606h2.cif
_cod_data_source_block           KubASCF3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Orange' changed to 'orange'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037964--7037965.cif.
;
_cod_original_formula_sum        'C22 H22 Cl2 F6 Ir N2 O0.50'
_cod_database_code               7037965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1S-H1SB = O1S-H1SA
 0.95 with sigma of 0.02
 H1SA-H1SB
 1.5 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C1'(H1'), C2'(H2'),
 C4'(H4'), C7'(H7'), C9'(H9'), C10'(H10')
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C18'(H18D,H18E,H18F), C19'(H19D,H19E,H19F),
 C20'(H20D,H20E,H20F), C21'(H21D,H21E,H21F), C22'(H22D,H22E,H22F)
;
_shelx_res_checksum              82850
_shelx_fab_checksum              55445
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'