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_4130632
_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         'C192 H144 Co4 N36, 12(F6 P)'
_chemical_formula_sum            'C250 H231 Co4 F72 N65 P12'
_chemical_formula_weight         6121.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6723(3)
_cell_length_b                   38.7772(8)
_cell_length_c                   38.7947(6)
_cell_measurement_reflns_used    32595
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      50.6310
_cell_measurement_theta_min      3.5010
_cell_volume                     28071.1(9)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
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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)'
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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -27.00   69.00   0.3000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 320

  2 omega  -23.00   73.00   0.3000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 320

  3 omega  -70.00   26.00   0.3000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 320

  4 omega  -86.00  -35.00   0.3000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   90.0000 170

  5 omega   23.00  116.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647 -125.0000    0.0000 310

  6 omega   27.00  138.90   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647   20.0000  121.0000 373

  7 omega  -12.00   93.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647  -77.0000    0.0000 350

  8 omega   -9.00   87.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647  -57.0000   30.0000 320

  9 omega   23.00  116.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647 -125.0000 -150.0000 310

 10 omega   -9.00   85.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647  -57.0000 -180.0000 314

 11 omega   37.00  123.10   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647   57.0000  -30.0000 287

 12 omega   38.00  131.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647   57.0000 -180.0000 310

 13 omega   88.00  116.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega   19.00   82.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       61.4647  -38.0000 -180.0000 210
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0359603000
_diffrn_orient_matrix_UB_12      0.0315311000
_diffrn_orient_matrix_UB_13      0.0161578000
_diffrn_orient_matrix_UB_21      -0.0398715000
_diffrn_orient_matrix_UB_22      -0.0240182000
_diffrn_orient_matrix_UB_23      0.0244938000
_diffrn_orient_matrix_UB_31      0.0627312000
_diffrn_orient_matrix_UB_32      0.0028341000
_diffrn_orient_matrix_UB_33      0.0267748000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            116463
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        38.078
_diffrn_reflns_theta_max         38.078
_diffrn_reflns_theta_min         3.224
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.447
_exptl_absorpt_correction_T_max  0.978
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_exptl_absorpt_correction_type   gaussian
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;
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            red
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_exptl_crystal_density_diffrn    1.448
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_exptl_crystal_F_000             12488
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diisopropyl ether by vapour diffusion'
_exptl_crystal_size_max          0.2919
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15031
_refine_ls_number_restraints     1200
_refine_ls_restrained_S_all      3.249
_refine_ls_R_factor_all          0.2040
_refine_ls_R_factor_gt           0.1725
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4398
_refine_ls_wR_factor_ref         0.4577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10625
_reflns_number_total             15031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05364_si_001.cif
_cod_data_source_block           pl15004
_cod_database_code               4130632
_chemical_oxdiff_formula         'C96 H72 Co2 F36 N18 P6'
_chemical_oxdiff_usercomment     '@ 120 K MB2170'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
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_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. Restrained distances
 N33-C168 \\sim N21-C103 \\sim N6-C26 \\sim N3-C7 \\sim N9-C39 \\sim N12-C58
\\sim N24-C122 \\sim N27-C136
 \\sim N30-C155 \\sim N36-C187 \\sim N18-C90 \\sim N15-C71
 with sigma of 0.02
3. 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
 P4, F19, F20, F21, F22, F23, F24
 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
 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
4. Same fragment restrains
{P1, F5, F2, F1, F4, F3, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P3, F13, F14, F15, F16, F17, F18}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P6, F31, F32, F33, F34, F35, F36}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P7, F37, F38, F39, F40, F41, F42}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P8, F43, F44, F45, F46, F47, F48}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P8A, F43A, F44A, F45A, F46A, F47A, F48A}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P9, F49, F50, F51, F52, F53, F54}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P10, F55, F56, F57, F58, F59, F60}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P11, F61, F62, F63, F64, F65, F66}
{P1, F5, F2, F1, F4, F3, F6} sigma for 1-2: 0.02, 1-3: 0.02
as
{P12, F67, F68, F69, F70, F71, F72}
5. Others
 Sof(P8A)=Sof(F43A)=Sof(F44A)=Sof(F45A)=Sof(F46A)=Sof(F47A)=Sof(F48A)=1-FVAR(1)
 Sof(P8)=Sof(F43)=Sof(F44)=Sof(F45)=Sof(F46)=Sof(F47)=Sof(F48)=FVAR(1)
6.a Fixed occupancy and ADP/Uiso:
 F31, F32, F33, F34, F35, F36, F37, F38, F39, F40, F41, F42, F43, F44, F45,
 F46, F47, F48, F43A, F44A, F45A, F46A, F47A, F48A, F49, F50, F51, F52, F53,
 F54, F55, F56, F57, F58, F59, F60, F61, F62, F63, F64, F65, F66, F67, F68, F69,
  F70, F71, F72
6.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C58(H58A,H58B,
 H58C), C71(H71A,H71B,H71C), C90(H90A,H90B,H90C), C103(H10A,H10B,H10C),
 C122(H12A,H12B,H12C), C136(H13A,H13B,H13C), C155(H15A,H15B,H15C), C168(H16A,
 H16B,H16C), C187(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C134(H134), C133(H133), C132(H132), C131(H131), C150(H150), C151(H151),
 C152(H152), C153(H153), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C29(H29), C30(H30), C32(H32), C34(H34), C35(H35), C36(H36),
 C37(H37), C42(H42), C43(H43), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C61(H61), C62(H62), C63(H63),
 C66(H66), C67(H67), C68(H68), C69(H69), C74(H74), C75(H75), C77(H77), C79(H79),
  C80(H80), C82(H82), C83(H83), C85(H85), C86(H86), C87(H87), C88(H88),
 C93(H93), C94(H94), C96(H96), C101(H101), C100(H100), C99(H99), C98(H98),
 C106(H106), C107(H107), C109(H109), C111(H111), C112(H112), C114(H114),
 C115(H115), C117(H117), C118(H118), C119(H119), C120(H120), C125(H125),
 C126(H126), C128(H128), C139(H139), C140(H140), C142(H142), C148(H148),
 C147(H147), C145(H145), C144(H144), C158(H158), C159(H159), C161(H161),
 C163(H163), C164(H164), C165(H165), C166(H166), C171(H171), C172(H172),
 C174(H174), C176(H176), C177(H177), C179(H179), C180(H180), C182(H182),
 C183(H183), C184(H184), C185(H185), C190(H190), C191(H191), C193(H193)
6.d Fitted pentagon refined as free rotating group:
 N21(C104,N20,C97,C102), N29(C156,N30,C154,C149)
6.e Fitted hexagon refined as free rotating group:
 C135(C134,C133,C132,C131,C130), C61(C62,C64,C63,N10,C60), C78(C79,C80,C81,C82,
 C83), C110(C111,C112,C113,C114,C115), C124(C125,C126,C127,C128,N22), C143(C148,
 C147,C146,C145,C144)
;
_shelx_res_checksum              26885
_shelx_hkl_checksum              90363
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_submission_special_instructions 'No special instructions were received'