Orthogonal Selection and Fixing of Coordination Self-Assembly Pathways for Robust Metallo-organic Ensemble Construction.
Burke, Michael J.; Nichol, Gary S.; Lusby, Paul J.; Journal of the American Chemical Society 138 (2016) 9308–9315; doi:10.1021/jacs.6b05364

data_4130630
_publ_section_title
;
 Orthogonal Selection and Fixing of Coordination Self-Assembly Pathways
 for Robust Metallo-organic Ensemble Construction.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9308
_journal_page_last               9315
_journal_paper_doi               10.1021/jacs.6b05364
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C84 H66 Co2 N12, 6(B F4), 6 C2 H3 N'
_chemical_formula_sum            'C96 H84 B6 Co2 F24 N18'
_chemical_formula_weight         2128.53
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   17.3577(3)
_cell_length_b                   17.3577(3)
_cell_length_c                   104.263(2)
_cell_measurement_reflns_used    16813
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.6480
_cell_measurement_theta_min      4.4730
_cell_volume                     27204.8(8)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
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_diffrn_measurement_details
;
  1 omega -122.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -19.0000    0.0000 115

  2 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000  -30.0000 79

  3 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000 -180.0000 79

  4 omega  -95.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  125.0000 -150.0000 93

  5 omega   23.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4186 -125.0000   60.0000 75

  6 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

  7 omega   89.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   35.0000  -27.9067 89

  8 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

  9 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -90.0000 84

 10 omega   37.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -90.0000 105

 11 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 55

 12 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   30.0000 91

 13 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 79

 14 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

 15 omega   40.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 59

 16 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

 17 omega   40.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 59

 18 omega   31.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  -30.0000 125

 19 omega   84.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   59.0000 -128.0272 94

 20 omega   37.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -90.0000 105

 21 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 82

 22 omega   40.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 59

 23 omega   40.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 59

 24 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 82

 25 omega   40.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 59

 26 omega   31.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  120.0000 125

 27 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

 28 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 82

 29 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -120.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0997358000
_diffrn_orient_matrix_UB_12      -0.0354876000
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_diffrn_orient_matrix_UB_21      0.0241529000
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_diffrn_orient_matrix_UB_31      0.0000389000
_diffrn_orient_matrix_UB_32      0.0648854000
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_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_limit_l_min       -108
_diffrn_reflns_number            81531
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.410
_diffrn_reflns_theta_max         53.410
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.4717
_exptl_absorpt_correction_T_min  0.2772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1474 before and 0.0980 after correction.
The Ratio of minimum to maximum transmission is 0.5877.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.559
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_exptl_crystal_F_000             13032
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diisopropyl ether by vapour diffusion'
_exptl_crystal_size_max          0.1618
_exptl_crystal_size_mid          0.1049
_exptl_crystal_size_min          0.0623
_platon_squeeze_details          '6 MeCN per asymmetric unit'
_refine_diff_density_max         1.855
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1247P)^2^+272.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2137
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3030
_reflns_number_total             3562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05364_si_004.cif
_cod_data_source_block           pl15025
_cod_original_cell_volume        27204.8(11)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4130630
_chemical_oxdiff_formula         'C84 H66 Co2 F3 N12 P6'
_chemical_oxdiff_usercomment     '@ 120 K MB3170-BF4'
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C12(H12), C28(H28), C8(H8), C15(H15), C2(H2), C7(H7),
 C25(H25), C4(H4), C22(H22), C26(H26), C3(H3), C20(H20), C21(H21), C19(H19)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              97183
_shelx_hkl_checksum              70052
_shelx_fab_checksum              23769
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-01
_olex2_date_sample_submission    2015-09-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id MB3170-BF4
_olex2_submission_special_instructions 'No special instructions were received'