A metal-organic framework supported iridium catalyst for the gas phase hydrogenation of ethylene.
Perlata, Ricardo A.; Huxley, Michael T.; Shi, Zhaolin; Zhang, Yue-Biao; Sumby, Christopher J.; Doonan, Christian J.; Chemical communications (Cambridge, England) 56 (2020) 15313–15316; doi:10.1039/d0cc06058e

data_7127600
_publ_section_title
;
 A metal-organic framework supported iridium catalyst for the gas phase
 hydrogenation of ethylene.
;
_journal_issue                   97
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15313
_journal_page_last               15316
_journal_paper_doi               10.1039/d0cc06058e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C76 H68 Cl0.5 Ir0.6 Mn3 N12 O12, 0.1(Cl)'
_chemical_formula_sum            'C90.88 H116.1 Cl0.6 Ir0.6 Mn3 N12 O20.02'
_chemical_formula_weight         1998.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-02 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.364(3)
_cell_length_b                   33.500(7)
_cell_length_c                   12.912(3)
_cell_measurement_reflns_used    68881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.048
_cell_measurement_theta_min      1.216
_cell_volume                     5305(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.750
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.750
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            67414
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.912
_diffrn_reflns_theta_min         1.216
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             2074
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The structure contains large solvent accessible voids containing
disordered solvent, in this case ethanol. To account for the 
removed electron density, 8 ethanol molecules (26e) per 
formula unit were added to the formula (16 ethanol molecules
per unit cell).
;
_refine_diff_density_max         1.710
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10667
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0924
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3047
_refine_ls_wR_factor_ref         0.3129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8625
_reflns_number_total             10667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06058e2.cif
_cod_data_source_block           MnMOF-1-IrClrev
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5304.8(19)
_cod_original_formula_sum        'C90.88 H116.10 Cl0.60 Ir0.60 Mn3 N12 O20.02'
_cod_database_code               7127600
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.733
_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
2. Restrained distances
 N62A-Ir3A
 2.15 with sigma of 0.02
 Ir3B-C85
 2.25 with sigma of 0.02
 Ir3B-C86
 2.25 with sigma of 0.02
 C85-C86
 1.3 with sigma of 0.02
 C85-C85_$1
 -2.6 with sigma of 0.02
 C63A-C66A
 1.54 with sigma of 0.02
 C65B-C67B
 -1.5 with sigma of 0.02
 C63B-C66B
 1.54 with sigma of 0.02
 N61B-C65B
 1.35 with sigma of 0.02
 N62B-C51B
 1.45 with sigma of 0.02
 C51A-N61A
 1.45 with sigma of 0.02
 N61A-N62A
 1.35 with sigma of 0.02
 C63A-C64A
 1.35 with sigma of 0.02
 C65A-C67A
 1.54 with sigma of 0.02
3. Restrained planarity
 C71A, C72A, C73A, C74A, C75A, C76A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C51A \\sim N61A \\sim N62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim
C67A \\sim N61B \\sim C65B \\sim C64B \\sim C63B \\sim C67B \\sim C71A \\sim
C72A \\sim C73A \\sim C74A \\sim C75A \\sim C76A \\sim Ir3A \\sim Ir3B \\sim
Cl81 \\sim Cl82: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(C85) = Uiso(C86)
5. Same fragment restrains
{C51B, N62B, N61B, C65B, C64B, C63B, C67B, C66B, C71B, C72B, C73B, C74B, C75B,
C76B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C51A, N61A, N62A, C63A, C64A, C65A, C66A, C67A, C71A, C72A, C73A, C74A, C75A,
C76A}
6. Others
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=
 Sof(H26B)=1-FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(H26A)=FVAR(1)
 Fixed Sof: C51B(0.375) H51A(0.375) H51B(0.375) N62B(0.75) N61B(0.75)
 C65B(0.75) C64B(0.75) C63B(0.75) C67B(0.75) H67A(0.75) H67B(0.75) H67C(0.75)
 C66B(0.75) H66A(0.75) H66B(0.75) H66C(0.75) C71B(0.75) C72B(0.75) H72B(0.75)
 C73B(0.75) H73B(0.75) C74B(0.75) C75B(0.75) H75B(0.75) C76B(0.75) H76B(0.75)
 C51A(0.125) H51C(0.125) H51D(0.125) N61A(0.25) N62A(0.25) C63A(0.25)
 C64A(0.25) C65A(0.25) C66A(0.25) H66D(0.25) H66E(0.25) H66F(0.25) C67A(0.25)
 H67D(0.25) H67E(0.25) H67F(0.25) C71A(0.25) C72A(0.25) H72A(0.25) C73A(0.25)
 H73A(0.25) C74A(0.25) C75A(0.25) H75A(0.25) C76A(0.25) H76A(0.25) Ir3A(0.05)
 Ir3B(0.25) Cl82(0.25) C85(0.25) H85A(0.25) H85B(0.25) Cl81(0.05) C86(0.25)
 H86A(0.25) H86B(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C51B(H51A,H51B), C51A(H51C,H51D), C85(H85A,H85B), C86(H86A,H86B)
7.b Aromatic/amide H refined with riding coordinates:
 C22A(H22A), C22B(H22B), C23A(H23A), C23B(H23B), C25A(H25A), C25B(H25B),
 C26A(H26A), C26B(H26B), C42(H42), C43(H43), C45(H45), C46(H46), C72B(H72B),
 C73B(H73B), C75B(H75B), C76B(H76B), C72A(H72A), C73A(H73A), C75A(H75A),
 C76A(H76A)
7.c Fitted hexagon refined as free rotating group:
 C71B(C72B,C73B,C74B,C75B,C76B)
7.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C67B(H67A,H67B,H67C), C66B(H66A,H66B,H66C), C66A(H66D,H66E,H66F),
 C67A(H67D,H67E,H67F)
;
_shelx_res_checksum              31931
_shelx_fab_checksum              9697
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20