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_4130629
_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
'C78 H54 Co2 N12, 6(B F4), 0.5(H2 O), 7(C2 H3 N)'
_chemical_formula_sum            'C92 H76 B6 Co2 F24 N19 O0.5'
_chemical_formula_weight         2094.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                73.1727(12)
_cell_angle_beta                 68.6423(12)
_cell_angle_gamma                80.3164(11)
_cell_formula_units_Z            2
_cell_length_a                   15.00712(20)
_cell_length_b                   16.8669(2)
_cell_length_c                   20.4390(3)
_cell_measurement_reflns_used    76965
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      76.0720
_cell_measurement_theta_min      3.6900
_cell_volume                     4600.53(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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    '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 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

  2 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -180.0000 96

  3 omega  -70.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000  -30.0000 97

  4 omega  -75.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   77.0000   60.0000 106

  5 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   77.0000 -180.0000 105

  6 omega    1.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000   60.0000 82

  7 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 55

  8 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

  9 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -90.0000 84

 10 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 59

 11 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 59

 12 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 13 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 82

 14 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 82

 15 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

 16 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  150.0000 91

 17 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   33.0000  -78.7191 90

 18 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 59

 19 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 91

 20 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

 21 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

 22 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -60.0000 84

 23 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

 24 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   30.0000 84

 25 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000   30.0000 98

 26 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 79

 27 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -30.0000 84

 28 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 91

 29 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -90.0000 98

 30 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -90.0000 59

 31 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

 32 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

 33 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

 34 omega -116.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000  -60.0000 95

 35 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  -90.0000 105

 36 omega -116.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -180.0000 95

 37 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   60.0000 96

 38 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

 39 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000    0.0000 105

 40 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  150.0000 105

 41 omega    1.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000 -150.0000 82

 42 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000  -71.7538 96

 43 omega   80.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 41

 44 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 95

 45 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 98

 46 omega   85.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   56.0000 -130.8423 93

 47 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 95

 48 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 95

 49 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   66.0000   28.5098 96

 50 omega   84.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   57.0000  -32.4247 94

 51 omega   81.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   72.0000  173.1406 97

 52 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 95

 53 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 95

 54 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 95

 55 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 95

 56 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -150.0000 91

 57 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000  113.6467 95

 58 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000  -15.4858 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0731913000
_diffrn_orient_matrix_UB_12      0.0757275000
_diffrn_orient_matrix_UB_13      0.0059377000
_diffrn_orient_matrix_UB_21      -0.0661309000
_diffrn_orient_matrix_UB_22      -0.0417706000
_diffrn_orient_matrix_UB_23      -0.0206848000
_diffrn_orient_matrix_UB_31      -0.0497982000
_diffrn_orient_matrix_UB_32      -0.0408824000
_diffrn_orient_matrix_UB_33      0.0807360000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            151138
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.249
_diffrn_reflns_theta_min         3.163
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             2130
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile, diisopropyl ether and water by vapour diffusion'
_exptl_crystal_size_max          0.2679
_exptl_crystal_size_mid          0.2029
_exptl_crystal_size_min          0.0805
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00098(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1382
_refine_ls_number_reflns         19157
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0996P)^2^+3.9084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17903
_reflns_number_total             19157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05364_si_003.cif
_cod_data_source_block           pl15013
_cod_original_cell_volume        4600.52(11)
_cod_original_formula_sum        'C92 H76 B6 Co2 F24 N19 O0.50'
_cod_database_code               4130629
_chemical_oxdiff_formula         'C78 H54 Co2 F36 N12 P6'
_chemical_oxdiff_usercomment     '@ 120 K MB3069'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 F9-F10 \\sim F9-F11 \\sim F10-F11 \\sim F10A-F11A \\sim F10A-F9A \\sim F11A-F9A
 with sigma of 0.04
 B3-F9 \\sim B3-F10 \\sim B3-F11 \\sim B3-F12 \\sim B3-F10A \\sim B3-F11A \\sim
B3-F9A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F9, F9A, F10, F10A, F11, F11A, F12, B3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, F14, F15, F16, B4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F21A, F22A, F23A, F24A, B6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{F23, F22, F24, F21, B6} sigma for 1-2: 0.02, 1-3: 0.02
as
{F21A, F22A, F23A, F24A, B6A}
5. Others
 Sof(F9A)=Sof(F10A)=Sof(F11A)=1-FVAR(1)
 Sof(F9)=Sof(F10)=Sof(F11)=FVAR(1)
 Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(B6A)=1-FVAR(2)
 Sof(F23)=Sof(F22)=Sof(F24)=Sof(F21)=Sof(B6)=FVAR(2)
 Fixed Sof: O1(0.5) H1A(0.5) H1B(0.5)
6.a Free rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
 C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C59(H59), C60(H60), C62(H62), C64(H64), C65(H65), C67(H67), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C75(H75), C76(H76), C78(H78)
6.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              5230
_shelx_hkl_checksum              33950
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-08-07
_olex2_date_sample_submission    2015-08-05
_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 MB3069
_olex2_submission_special_instructions 'No special instructions were received'