Cyclometalated Ir-Zr Metal-Organic Frameworks as Recyclable Visible-Light Photocatalysts for Sulfide Oxidation into Sulfoxide in Water.
Wei, Lian-Qiang; Ye, Bao-Hui; ACS applied materials & interfaces  (2019) –; doi:10.1021/acsami.9b15646

data_4514433
_publ_section_title
;
 Cyclometalated Ir-Zr Metal-Organic Frameworks as Recyclable Visible-Light
 Photocatalysts for Sulfide Oxidation into Sulfoxide in Water.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.9b15646
_journal_year                    2019
_chemical_formula_moiety         'C46 H32 Ir N4 O4, Cl, 2(C H Cl3)'
_chemical_formula_sum            'C48 H34 Cl7 Ir N4 O4'
_chemical_formula_weight         1171.14
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                111.040(5)
_cell_angle_beta                 95.372(5)
_cell_angle_gamma                97.958(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3217(9)
_cell_length_b                   13.7563(7)
_cell_length_c                   16.7397(8)
_cell_measurement_reflns_used    4299
_cell_measurement_temperature    298
_cell_measurement_theta_max      59.9090
_cell_measurement_theta_min      3.4950
_cell_volume                     2591.0(3)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23039
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        64.966
_diffrn_reflns_theta_max         64.966
_diffrn_reflns_theta_min         3.503
_exptl_absorpt_coefficient_mu    8.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8738
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7398
_reflns_number_total             8738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b15646_si_002.cif
_cod_data_source_block           3
_cod_database_code               4514433
_shelx_shelxl_version_number     2014/7
_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
2. Restrained distances
 O1-C17
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl5) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(Cl6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a :
 N2(C18,C19,C20,C21,C22,C23,C24,C25,C26), N4(C36,C37,C38,C39,C40,C41,C42,C43,
 C44), C3(N1,C1,C2,C4,C5,C6,C7,C8,C9)
4.b Ternary CH refined with riding coordinates:
 C47(H47), C48(H48)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12),
  C13(H13), C14(H14), C15(H15), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
4.d Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15), C27(C28,C29,C30,C31,C32)
4.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C46(H46A,H46B,H46C)
;