Encapsulation of an organometallic cationic catalyst by direct exchange into an anionic MOF
Grigoropoulos, Alexios; Whitehead, George F. S.; Perret, Noémie; Katsoulidis, Alexandros P.; Chadwick, F. Mark; Davies, Robert P.; Haynes, Anthony; Brammer, Lee; Weller, Andrew S.; Xiao, Jianliang; Rosseinsky, Matthew J.; Chem. Sci. 7 (2016) 2037–; doi:10.1039/C5SC03494A

data_1540656
_publ_section_title
;
 Encapsulation of an organometallic cationic catalyst by direct exchange
 into an anionic MOF
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2037
_journal_paper_doi               10.1039/C5SC03494A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C12 H4 In O8, 0.282(Co)'
_chemical_formula_sum            'C12 H4 Co0.28 In O8'
_chemical_formula_weight         407.57
_chemical_name_systematic        '[(Cp2Co)x(TEA)3-x][In3(BTC)4]'
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-22
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   20.4031(2)
_cell_length_b                   20.4031(2)
_cell_length_c                   20.4031(2)
_cell_measurement_reflns_used    8801
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8880
_cell_measurement_theta_min      2.8060
_cell_volume                     8493.53(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega -110.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000    0.0000 125

  2 omega -110.00 -107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  120.0000 3
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
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_diffrn_orient_matrix_UB_11      -0.0217787000
_diffrn_orient_matrix_UB_12      -0.0094666000
_diffrn_orient_matrix_UB_13      -0.0253709000
_diffrn_orient_matrix_UB_21      -0.0078534000
_diffrn_orient_matrix_UB_22      -0.0289718000
_diffrn_orient_matrix_UB_23      0.0175554000
_diffrn_orient_matrix_UB_31      -0.0259273000
_diffrn_orient_matrix_UB_32      0.0167226000
_diffrn_orient_matrix_UB_33      0.0160296000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0206
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_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12923
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.863
_diffrn_reflns_theta_min         2.824
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_description       block
_exptl_crystal_F_000             2359
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 689 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1157P)^2^+42.2245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2013
_reflns_Friedel_coverage         0.849
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                1585
_reflns_number_total             1686
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_cod_data_source_file            c5sc03494a2.cif
_cod_data_source_block           c4_aga_cob_tea_3d_2
_cod_depositor_comments
'Adding full bibliography for 1540655--1540656.cif.'
_cod_original_cell_volume        8493.6(3)
_cod_database_code               1540656
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007)
;
_shelx_res_checksum              24668
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'