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_4131170
_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 H79 Cu N3 O, F6 P'
_chemical_formula_sum            'C79 H79 Cu F6 N3 O P'
_chemical_formula_weight         1294.96
_chemical_name_common            Cu-ISOCN-2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.737(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.4955(14)
_cell_length_b                   17.5041(6)
_cell_length_c                   27.6236(10)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      2.33
_cell_volume                     17038.9(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            80748
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        20.816
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         1.156
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.2565
_exptl_absorpt_correction_T_min  0.2046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1350 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.7977.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_description       block
_exptl_crystal_F_000             5440
_exptl_crystal_recrystallization_method 'see text'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         8922
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.0999
_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          0.2839
_refine_ls_wR_factor_ref         0.3390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5638
_reflns_number_total             8922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10460_si_002.cif
_cod_data_source_block           jfig1253
_cod_database_code               4131170
_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
 P1-F6 = P1-F5 = P1-F4 = P1-F2 = P1-F3 = P1-F1
 1.69967 with sigma of 0.02
 F1-F2 = F1-F5 = F1-F3 = F1-F6 = F4-F5 = F4-F6 = F4-F2 = F4-F3 = F3-F5 = F5-F6
 2.35078 with sigma of 0.02
 P1-F6A = P1-F5A = P1-F4A = P1-F2A = P1-F3A = P1-F1A
 1.69967 with sigma of 0.02
 F1A-F2A = F1A-F5A = F1A-F3A = F1A-F6A = F4A-F5A = F4A-F6A = F4A-F2A = F4A-F3A
 = F3A-F5A = F5A-F6A = F2A-F6A
 2.35078 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F2) = Uanis(F3) = Uanis(F4) = Uanis(F1) = Uanis(F5) =
Uanis(F4A) = Uanis(F3A) = Uanis(F5A) = Uanis(F1A) = Uanis(F2A) = Uanis(F6A)
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=FVAR(2)
 Sof(F4A)=Sof(F3A)=Sof(F5A)=Sof(F1A)=Sof(F2A)=Sof(F6A)=1-FVAR(3)
 Sof(F6)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F1)=Sof(F5)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB), C1BA(H1BA,H1BB), C7BA(H7BA,H7BB)
5.b Aromatic/amide H refined with riding coordinates:
 C61(H61), C33(H33), C11(H11), C35(H35), C57(H57), C7AA(H7AA), C65(H65),
 C44(H44), C0BA(H0BA), C19(H19), C41(H41), C68(H68), C1AA(H1AA), C76(H76),
 C74(H74), C9(H9), C14(H14), C1(H1), C2(H2)
5.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C46(H46A,H46B,H46C), C43(H43A,H43B,H43C), C39(H39A,H39B,
 H39C), C18(H18A,H18B,H18C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C21(H21A,
 H21B,H21C), C78(H78A,H78B,H78C), C5AA(H5AA,H5AB,H5AC), C69(H69A,H69B,H69C),
 C75(H75A,H75B,H75C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              90018
_shelx_hkl_checksum              76345
_shelx_fab_checksum              86985
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig1253
_olex2_submission_special_instructions 'No special instructions were received'