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_1540655
_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, C10 H10 Co'
_chemical_formula_sum            'C22 H14 Co In O8'
_chemical_formula_weight         580.08
_chemical_name_systematic        '[Cp2Co]3[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             2015-08-05
_audit_creation_method
;
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                   20.44700(10)
_cell_length_b                   20.44700(10)
_cell_length_c                   20.44700(10)
_cell_measurement_temperature    100(2)
_cell_volume                     8548.48(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47182
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.572
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88042
_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    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.046(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0868P)^2^+2.6458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.854
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                1916
_reflns_number_total             2012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03494a2.cif
_cod_data_source_block           test_new_rered_a
_cod_depositor_comments
'Adding full bibliography for 1540655--1540656.cif.'
_cod_original_cell_volume        8548.48(13)
_cod_database_code               1540655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1B-Co00
 2.03 with sigma of 0.02
 C1C-Co00
 2.03 with sigma of 0.02
 C1A-Co00
 2.03 with sigma of 0.02
 C1-Co00
 2.03 with sigma of 0.02
 C1D-Co00
 2.03 with sigma of 0.02
 C7-Co00
 2.03 with sigma of 0.02
 C3-Co00
 2.03 with sigma of 0.02
 C1AA-Co00
 2.03 with sigma of 0.02
 C2A-Co00
 2.03 with sigma of 0.02
 C2-Co00
 2.03 with sigma of 0.02
 C1D-C2A
 3.27 with sigma of 0.02
 C1C-C1AA
 3.27 with sigma of 0.02
 C1B-C3
 3.27 with sigma of 0.02
 C1A-C7
 3.27 with sigma of 0.02
 C1-C2
 3.27 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1A, Co00, C2, C2A, C7, C1, C1AA, C1D, C3, C1B, C1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Fixed Sof: Co00(0.25) C2(0.25) H2(0.25) C2A(0.25) H2A(0.25) C1AA(0.25)
 H1AA(0.25) C3(0.25) H3(0.25) C7(0.25) H7(0.25) C1C(0.25) H1C(0.25) C1D(0.25)
 H1D(0.25) C1(0.25) H1(0.25) C1A(0.25) H1A(0.25) C1B(0.25) H1B(0.25)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C2A(H2A), C1AA(H1AA), C1C(H1C), C1D(H1D), C1(H1), C1A(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C7(H7), C1B(H1B)
5.c Fitted pentagon refined as free rotating group:
 C2(C2A,C1AA,C3,C7), C1C(C1D,C1,C1A,C1B)
;
_shelx_res_checksum              24148
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'