A metal‒organic framework immobilised iridium pincer complex
Rimoldi, Martino; Nakamura, Akitake; Vermeulen, Nicolaas A.; Henkelis, James J.; Blackburn, Anthea K.; Hupp, Joseph T.; Stoddart, J. Fraser; Farha, Omar K.; Chem. Sci. 7 (2016) 4980–; doi:10.1039/C6SC01376G

data_1543293
_publ_section_title
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 A metal--organic framework immobilised iridium pincer complex
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_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4980
_journal_paper_doi               10.1039/C6SC01376G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C22 H38 Cl Ir O3 P2'
_chemical_formula_sum            'C22 H38 Cl Ir O3 P2'
_chemical_formula_weight         640.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-13
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_audit_update_record
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2016-03-14 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 106.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8099(3)
_cell_length_b                   20.1079(5)
_cell_length_c                   13.9635(4)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.573
_cell_measurement_theta_min      4.397
_cell_volume                     2636.11(13)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21915
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.605
_diffrn_reflns_theta_max         67.605
_diffrn_reflns_theta_min         3.972
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    12.035
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0572 before and 0.0387 after correction.
The Ratio of minimum to maximum transmission is 0.7708.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.021
_refine_diff_density_max         2.243
_refine_diff_density_min         -2.417
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0711
_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^)+54.8753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4512
_reflns_number_total             4681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01376g2.cif
_cod_data_source_block           p21-n
_cod_depositor_comments          'Adding full bibliography for 1543293.cif.'
_cod_database_code               1543293
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.417
_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) groups
2. Restrained distances
 C20-C19A = C19B-C11
 1.55 with sigma of 0.01
 C17-C15 \\sim C16-C15 \\sim C18-C15 \\sim C21-C20 \\sim C20-C13B \\sim
C22A-C20 \\sim C20-C14A \\sim C12-
 C11 \\sim C14-C11 \\sim C13A-C11 \\sim C8-C7 \\sim C7-C10 \\sim C9-C7
 with sigma of 0.02
 C22B-C11 \\sim C14-C11
 with sigma of 0.02
 C21-C13B \\sim C13B-C14A
 with sigma of 0.02
 C21-C22A \\sim C12-C22B
 with sigma of 0.02
 C12-C13A \\sim C13A-C14
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1A)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C22B)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(Cl1)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C19A(H19A,H19B), C19B(H19C,H19D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,
 H14E,H14F), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
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_olex2_submission_special_instructions 'No special instructions were received'