Iridium complexes catalysed the selective dehydrogenation of glucose to gluconic acid in water
Borja, Pilar; Vicent, Cristian; Baya, Miguel; García, Hermenegildo; Mata, Jose A.; Green Chemistry 20 (2018) 4094–; doi:10.1039/C8GC01933A

data_7231348
_publ_section_title
;
 Iridium complexes catalysed the selective dehydrogenation of glucose to
 gluconic acid in water
;
_journal_issue                   17
_journal_name_full               'Green Chemistry'
_journal_page_first              4094
_journal_paper_doi               10.1039/C8GC01933A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C15 H27 Ir N2 O2, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C18 H29 Cl2 F6 Ir N2 O8 S2'
_chemical_formula_weight         842.65
_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             2018-04-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.582(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2529(5)
_cell_length_b                   21.6653(7)
_cell_length_c                   12.9575(5)
_cell_measurement_reflns_used    22946
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      29.0080
_cell_measurement_theta_min      3.1320
_cell_volume                     2937.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -100.00 -55.00   0.50    2.50    --  -11.28 178.00  60.00   90
  2  \w    -20.00  31.00   0.50    2.50    --  -11.28 -99.00   0.00  102
  3  \w    -64.00  38.00   0.50    2.50    --   12.14 -37.00-150.00  204
  4  \w    -17.00  86.00   0.50    2.50    --   12.14  57.00 -60.00  206
  5  \w    -34.00  94.00   0.50    2.50    --   12.14  19.00  30.00  256
  6  \w    -20.00  31.00   0.50    2.50    --  -11.28 -99.00  30.00  102
  7  \w    -74.00 -29.00   0.50    2.50    --  -11.28 133.00  34.98   90
  8  \w     35.00  86.00   0.50    2.50    --   12.14 178.00 150.00  102
  9  \w      3.00  70.00   0.50    2.50    --   12.14-126.00 -66.30  134
 10  \w    -14.00  88.00   0.50    2.50    --   12.14  37.00-150.00  204
 11  \w     34.00 101.00   0.50    2.50    --   12.14-178.00  90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0660795000
_diffrn_orient_matrix_UB_12      -0.0058662000
_diffrn_orient_matrix_UB_13      -0.0283385000
_diffrn_orient_matrix_UB_21      0.0141141000
_diffrn_orient_matrix_UB_22      -0.0308715000
_diffrn_orient_matrix_UB_23      -0.0097524000
_diffrn_orient_matrix_UB_31      -0.0052806000
_diffrn_orient_matrix_UB_32      -0.0091932000
_diffrn_orient_matrix_UB_33      0.0506700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58882
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+9.4215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5442
_reflns_number_total             5992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc01933a3.cif
_cod_data_source_block           str2049
_cod_depositor_comments
'Adding full bibliography for 7231346--7231348.cif.'
_cod_original_cell_volume        2937.6(2)
_cod_database_code               7231348
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C47 H65 N2 O22 Ir S F'
_chemical_oxdiff_usercomment     'MB 226'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.2
Uanis(C19) \\sim Ueq: with sigma of 0.051 and sigma for terminal atoms of 0.2
Uanis(C18) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.2
Uanis(C12) = Uanis(C20)
Uanis(C19) = Uanis(C20)
Uanis(C12) = Uanis(C11)
3.a Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
3.c Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C12(H12A,H12B,
 H12C), C20(H20A,H20B,H20C)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
3.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              39123
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.351
_oxdiff_exptl_absorpt_empirical_full_min 0.762