Long-range metal‒ligand bifunctional catalysis: cyclometallated iridium catalysts for the mild and rapid dehydrogenation of formic acid
Barnard, Jonathan H.; Wang, Chao; Berry, Neil G.; Xiao, Jianliang; Chemical Science 4 (2013) 1234–; doi:10.1039/c2sc21923a

data_1514579
_publ_section_title
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 Long-range metal--ligand bifunctional catalysis: cyclometallated iridium
 catalysts for the mild and rapid dehydrogenation of formic acid
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              1234
_journal_paper_doi               10.1039/c2sc21923a
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H64 Cl Ir N2 O2, C6 H14'
_chemical_formula_sum            'C54 H78 Cl Ir N2 O2'
_chemical_formula_weight         1014.83
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-07-18
_audit_creation_method
;
Olex2 1.1-alpha
(compiled 2011.07.08 svn.r1848, GUI svn.r3697)
;
_audit_update_record
;
2012-05-31 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.5236(14)
_cell_length_b                   13.7422(8)
_cell_length_c                   14.3634(8)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.20
_cell_volume                     5038.0(5)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37760
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.743
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0768 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8023.
The \l/2 correction factor is 0.00.
{Info from C:\frames\Xiao\JBARNARD\JHB93\work\sad.abs}
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+8.5792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                10897
_reflns_number_total             11448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc21923a.txt
_cod_data_source_block           jhb93m
_cod_database_code               1514579