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_4131169
_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         'C79 H80 Cu N3 O, 4(C4 H8 O), F6 P'
_chemical_formula_sum            'C95 H112 Cu F6 N3 O5 P'
_chemical_formula_weight         1584.38
_chemical_name_common            Cu-ISOCN-3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 99.681(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.740(3)
_cell_length_b                   31.382(6)
_cell_length_c                   21.010(4)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.975
_cell_measurement_theta_min      2.831
_cell_volume                     8930(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.1341
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57062
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.817
_diffrn_reflns_theta_max         24.817
_diffrn_reflns_theta_min         1.298
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0916 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         15302
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.2176
_refine_ls_R_factor_gt           0.1230
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3287
_refine_ls_wR_factor_ref         0.3825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7686
_reflns_number_total             15302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10460_si_002.cif
_cod_data_source_block           jfig1246
_cod_database_code               4131169
_olex2_refinement_description
;
1. 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
2. Restrained distances
 P2-F5
 1.56 with sigma of 0.02
 C4-C5
 1.45 with sigma of 0.02
 C13S-C14S
 1.45 with sigma of 0.02
 O11S-C10S
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4S) = Uanis(C13S) = Uanis(C14S) = Uanis(C15S) = Uanis(C16S)
Uanis(C9S) = Uanis(C10S) = Uanis(O11S) = Uanis(C12S) = Uanis(C2S)
Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C02Y) = Uanis(O1)
Uanis(F1) = Uanis(F2) = Uanis(F5) = Uanis(F4) = Uanis(F3) = Uanis(F6)
Uanis(C6S) = Uanis(C5S) = Uanis(O3S) = Uanis(C8S) = Uanis(C7S)
4. Rigid body (RIGU) restrains
 F5, P2, F2, F1, F4, F3, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F8, F10, P1, F7, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C1S, C0AA, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: P1(0.5) P2(0.5) F3(0.5) F2(0.5) F12(0.5) F9(0.5) F10(0.5) F6(0.5)
 F8(0.5) F11(0.5) F4(0.5) F5(0.5) F7(0.5) F1(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C9S(H9SA,H9SB), C4S(H4SA,H4SB), C13S(H13A,H13B), C16S(H16A,
 H16B), C2S(H2SA,H2SB), C12S(H12A,H12B), C10S(H10A,H10B), C0AA(H0AA,H0AB),
 C3S(H3SA,H3SB), C14S(H14D,H14E), C02Y(H02A,H02B), C3(H3A,H3B), C5(H5A,H5B),
 C4(H4A,H4B), C15S(H15A,H15B), C5S(H5SA,H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB),
 C8S(H8SA,H8SB)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C54(H54), C74(H74), C67(H67), C34(H34), C32(H32), C15(H15),
 C71(H71), C18(H18), C27(H27), C50(H50), C47(H47), C24(H24), C59(H59), C42(H42),
  C39(H39), C62(H62)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C76(H76A,H76B,H76C), C70(H70A,H70B,H70C), C14(H14A,H14B,
 H14C), C17(H17A,H17B,H17C), C73(H73A,H73B,H73C), C29(H29A,H29B,H29C), C52(H52A,
 H52B,H52C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C), C58(H58A,H58B,H58C),
 C44(H44A,H44B,H44C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C49(H49A,H49B,
 H49C), C41(H41A,H41B,H41C), C64(H64A,H64B,H64C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              52549
_shelx_hkl_checksum              93288
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'