Non-equilibrium cobalt(iii) “click” capsules
Symmers, P. R.; Burke, M. J.; August, D. P.; Thomson, P. I. T.; Nichol, G. S.; Warren, M. R.; Campbell, C. J.; Lusby, P. J.; Chem. Sci. 6 (2015) 756–; doi:10.1039/C4SC03036B

data_1517951
_publ_section_title
;
 Non-equilibrium cobalt(iii) &#x201C;click&#x201D; capsules
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              756
_journal_paper_doi               10.1039/C4SC03036B
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C252 H276 Co4 N48, 6(F6 P)'
_chemical_formula_sum            'C252 H276 Co4 F36 N48 P6'
_chemical_formula_weight         5082.73
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   30.5162(6)
_cell_length_b                   30.5162(6)
_cell_length_c                   71.022(2)
_cell_measurement_reflns_used    26199
_cell_measurement_temperature    298
_cell_measurement_theta_max      22.4920
_cell_measurement_theta_min      1.5920
_cell_volume                     57278(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.335
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -60.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000    0.0000    0.0000 175

  2 omega  -60.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -50.0000    0.0000 120

  3 omega  -60.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -50.0000  120.0000 120

  4 omega  -60.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -50.0000  240.0000 120
;
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'omega rotation with 1 degree frames'
_diffrn_orient_matrix_UB_11      -0.0075661000
_diffrn_orient_matrix_UB_12      -0.0179916000
_diffrn_orient_matrix_UB_13      -0.0070314000
_diffrn_orient_matrix_UB_21      0.0194786000
_diffrn_orient_matrix_UB_22      0.0169750000
_diffrn_orient_matrix_UB_23      -0.0056210000
_diffrn_orient_matrix_UB_31      0.0155572000
_diffrn_orient_matrix_UB_32      -0.0082165000
_diffrn_orient_matrix_UB_33      0.0036250000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1625
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.335
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            54444
_diffrn_reflns_point_group_measured_fraction_full 0.335
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         16.681
_diffrn_reflns_theta_min         1.519
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.884
_exptl_crystal_description       block
_exptl_crystal_F_000             15876
_exptl_crystal_recrystallization_method
'From acetonitrile and diisopropyl ether.'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.553
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         7730
_refine_ls_number_restraints     1113
_refine_ls_restrained_S_all      1.537
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.1218
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3268
_refine_ls_wR_factor_ref         0.3455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6141
_reflns_number_total             7730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03036b2.cif
_cod_data_source_block           pl4001
_cod_depositor_comments          'Adding full bibliography for 1517951.cif.'
_cod_original_cell_volume        57278(3)
_cod_database_code               1517951
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C252 H276 Co4 F72 N48 P12'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.68
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. 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
3.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C11(H11), C35(H35), C37(H37), C42(H42), C46(H46), C48(H48),
 C53(H53), C77(H77), C79(H79), C84(H84)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C32(H32A,H32B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,
 H45B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C74(H74A,H74B), C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B),
  C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C23(H23),
 C24(H24), C26(H26), C27(H27), C29(H29), C31(H31), C54(H54), C57(H57), C58(H58),
  C60(H60), C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69),
 C70(H70), C73(H73)
;
_shelx_res_checksum              18336
_olex2_exptl_crystal_mounting_method 'Mitegen tip.'
_olex2_submission_original_sample_id MB-1-110
_olex2_submission_special_instructions 'No special instructions were received'