Hydrogen generation from formic acid decomposition on a highly efficient iridium catalyst bearing a diaminoglyoxime ligand
Lu, Sheng-Mei; Wang, Zhijun; Wang, Jijie; Li, Jun; Li, Can; Green Chemistry 20 (2018) 1835–; doi:10.1039/C8GC00495A

data_7230313
_publ_section_title
;
 Hydrogen generation from formic acid decomposition on a highly efficient
 iridium catalyst bearing a diaminoglyoxime ligand
;
_journal_issue                   8
_journal_name_full               'Green Chemistry'
_journal_page_first              1835
_journal_paper_doi               10.1039/C8GC00495A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C18 H29 Cl Ir N4 O2, Cl'
_chemical_formula_sum            'C18 H29 Cl2 Ir N4 O2'
_chemical_formula_weight         596.57
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                88.195(2)
_cell_angle_beta                 86.069(2)
_cell_angle_gamma                89.089(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1521(12)
_cell_length_b                   9.6810(12)
_cell_length_c                   11.7658(15)
_cell_measurement_reflns_used    3935
_cell_measurement_temperature    130
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.231
_cell_volume                     1039.4(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8434
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         1.736
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.701
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0872 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.7253.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_refine_diff_density_max         2.879
_refine_diff_density_min         -3.180
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             4763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc00495a2.cif
_cod_data_source_block           mo_dm16457_0m
_cod_depositor_comments          'Adding full bibliography for 7230313.cif.'
_cod_database_code               7230313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O1(H1), O2(H2), N2(H2A), N3(H3)
2.b Ternary CH refined with riding coordinates:
 C2(H2B), C3(H3A)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              999
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'