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_4130631
_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         'C168 H132 Co4 N24, 12(F6 P) + solvent'
_chemical_formula_sum            'C168 H132 Co4 F72 N24 P12'
_chemical_formula_weight         4462.33
_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             2015-09-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   20.5996(2)
_cell_length_b                   20.5996(2)
_cell_length_c                   195.2193(18)
_cell_measurement_reflns_used    20459
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.7010
_cell_measurement_theta_min      4.0030
_cell_volume                     71741.6(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, 2015)'
_diffrn_ambient_environment      air
_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
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega -123.00   -3.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3508  -77.0000   30.0000 400

  2 omega  -50.00   40.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3508   38.0000 -180.0000 300

  3 omega    1.00   82.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.3508  -99.0000 -120.0000 270

  4 omega   26.00  107.00   0.3000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.9147  -94.0000  150.0000 270

  5 omega   35.00   98.00   0.3000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.9147  -45.0000  120.0000 210

  6 omega   82.00  178.00   0.3000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.9147   45.0000  -90.0000 320

  7 omega   32.00   89.90   0.3000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.9147  -30.0000  -90.0000 193

  8 omega   32.00   89.90   0.3000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.9147  -30.0000  -60.0000 193

  9 omega  -50.00   40.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3508   38.0000   90.0000 300

 10 omega -124.00  -79.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3508  -99.0000  150.0000 150

 11 omega -123.00   -3.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3508  -77.0000 -180.0000 400
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0291250000
_diffrn_orient_matrix_UB_12      0.0781773000
_diffrn_orient_matrix_UB_13      -0.0031885000
_diffrn_orient_matrix_UB_21      0.0133026000
_diffrn_orient_matrix_UB_22      0.0345769000
_diffrn_orient_matrix_UB_23      0.0072200000
_diffrn_orient_matrix_UB_31      0.0801587667
_diffrn_orient_matrix_UB_32      0.0123842333
_diffrn_orient_matrix_UB_33      -0.0000370667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       244
_diffrn_reflns_limit_l_min       -238
_diffrn_reflns_number            97557
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.084
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59974
_exptl_absorpt_correction_type   multi-scan
_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)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       prism
_exptl_crystal_F_000             26928
_exptl_crystal_recrystallization_method
;
The material was recrystallised from a mixture of 
acetonitrile and diisopropyl ether by vapour diffusion
;
_exptl_crystal_size_max          0.2929
_exptl_crystal_size_mid          0.1942
_exptl_crystal_size_min          0.1924
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         16050
_refine_ls_number_restraints     526
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0911
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1981P)^2^+39.2358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2689
_refine_ls_wR_factor_ref         0.2877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11098
_reflns_number_total             16050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05364_si_002.cif
_cod_data_source_block           pl15015_sq
_cod_original_cell_volume        71741.6(15)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4130631
_chemical_oxdiff_formula         'C84 H66 Co2 F36 N12 P6'
_chemical_oxdiff_usercomment     '@ 120 K MB3067'
_diffrn_oxdiff_twin_integration_method simultaneous
_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. Shared sites
{C40, C40A}
{C41, C41A}
{C43, C43A}
{C44, C44A}
3. Restrained distances
 P6-F25 \\sim P6-F26 \\sim P6-F27 \\sim P5-F23 \\sim P5-F21 \\sim P5-F20 \\sim
P5-F22 \\sim P3-F16 \\sim P3-
 F17 \\sim P3-F18 \\sim P3-F13 \\sim P3-F14 \\sim P3-F15 \\sim P2-F10 \\sim
P2-F11 \\sim P2-F12 \\sim P2-F7 ~
 P2-F8 \\sim P2-F9 \\sim P1-F5 \\sim P1-F4 \\sim P1-F6 \\sim P1-F2 \\sim P1-F1
\\sim P1-F3 \\sim P4-F19
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C40) = Uanis(C40A)
Uanis(C41) = Uanis(C41A)
Uanis(C43) = Uanis(C43A)
Uanis(C44) = Uanis(C44A)
5. Rigid body (RIGU) restrains
 P3, F13, F14, F15, F16, F17, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P6, F25, F26, F27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46A, C40A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C40A)=Sof(C41A)=Sof(H41A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=
 Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Fixed Sof: F22(0.66667) F23(0.66667)
7.a Me refined with riding coordinates:
 C46A(H46D,H46E,H46F)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C13(H13), C16(H16),
 C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C38(H38), C40(H40),
 C43(H43), C41A(H41A), C44A(H44A), C47(H47), C49(H49), C50(H50), C53(H53),
 C54(H54), C55(H55), C56(H56)
7.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C45A(H45D,H45E,
 H45F), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              27027
_shelx_hkl_checksum              80591
_shelx_fab_checksum              94286
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-08-27
_olex2_date_sample_submission    2015-08-24
_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 MB3067
_olex2_submission_special_instructions 'No special instructions were received'