Robust, Transformable, and Crystalline Single-Node Organometallic Networks Constructed from Ditopic m-Terphenyl Isocyanides.
Agnew, Douglas W.; Gembicky, Milan; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Journal of the American Chemical Society 138 (2016) 15138–15141; doi:10.1021/jacs.6b10460

data_4131171
_publ_section_title
;
 Robust, Transformable, and Crystalline Single-Node Organometallic
 Networks Constructed from Ditopic m-Terphenyl Isocyanides.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15138
_journal_page_last               15141
_journal_paper_doi               10.1021/jacs.6b10460
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C100 H95 Cu N4, F6 P, 3(C4 H8 O)'
_chemical_formula_sum            'C112 H119 Cu F6 N4 O3 P'
_chemical_formula_weight         1777.61
_chemical_name_common            Cu-ISOCN-1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.4380(14)
_cell_length_b                   44.985(2)
_cell_length_c                   30.3992(14)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.975
_cell_measurement_theta_min      2.831
_cell_volume                     41624(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47645
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        59.037
_diffrn_reflns_theta_max         59.037
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'Micro Focus Rotating Anode'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.1523
_exptl_absorpt_correction_T_min  0.0623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1076 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.4091.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             15056
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 4649 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.284(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         14032
_refine_ls_number_restraints     614
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0887
_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^)+(0.1845P)^2^+135.6550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2476
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                11750
_reflns_number_total             14032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10460_si_002.cif
_cod_data_source_block           JFigCu157
_cod_original_cell_volume        41625(3)
_cod_database_code               4131171
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.534(4) 0.466(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 F2A-F3A
 2.056 with sigma of 0.02
 F5-F3
 2.05 with sigma of 0.02
 C97-C96
 1.5 with sigma of 0.02
 C8S-C7S = C6S-C7S = C6S-C5S
 1.55 with sigma of 0.01
 C11S-C12S
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
F6 \\sim F1 \\sim F2 \\sim F3 \\sim F5 \\sim F4 \\sim P1: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(O2S) \\sim Ueq, Uanis(C8S) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C66) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C60)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F5) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C03H) = Uanis(C96) = Uanis(C95)
5. Rigid body (RIGU) restrains
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3S, C9S, C10S, C11S, C12S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7S, C8S, O2S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C92, C93, C94, C95, C96, C97, C98, C03H
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C16, C11, C10, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C39, C34, C35, C40, C36, C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C61, C60, C59, C65, C58, C64, C63, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, C46, C41, C42, C49, C43, C44, C45, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C20, C21, C19, C18, C17, C22, C23, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8S, C5S, C6S, C7S, O2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: P1(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) P1A(0.5)
 F1A(0.5) F2A(0.5) F3A(0.5) F4A(0.5) F5A(0.5) F6A(0.5)
 Fixed X: H97A(0.55576) H97B(0.546169) H97C(0.59372)
 Fixed Y: H97A(0.052509) H97B(0.021211) H97C(0.02797)
 Fixed Z: H97A(0.39841) H97B(0.37533) H97C(0.39544)
7.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C9S(H9SA,
 H9SB), C10S(H10A,H10B), C11S(H11A,H11B), C12S(H12A,H12B), C7S(H7SA,H7SB),
 C8S(H8SA,H8SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB)
7.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C88(H88A,
 H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C98(H98A,H98B,H98C)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C12(H12), C19(H19), C21(H21), C27(H27), C34(H34),
 C36(H36), C45(H45), C43(H43), C54(H54), C56(H56), C60(H60), C62(H62), C70(H70),
  C72(H72), C77(H77), C81(H81), C84(H84), C86(H86), C94(H94), C03H(H03H)
7.d Fitted hexagon refined as free rotating group:
 C46(C45,C44,C43,C42,C41), C91(C92,C94,C95,C03H,C96)
7.e Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C)
;
_shelx_res_checksum              88578
_shelx_hkl_checksum              56248
_shelx_fab_checksum              34093
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'