Two-Dimensional and Three-Dimensional Coordination Polymers of Hexakis(4-cyanophenyl)[3]radialene: The Role of Stoichiometry and Kinetics
Hollis, Courtney A.; Batten, Stuart R.; Sumby, Christopher J.; Crystal Growth & Design 13 (2013) 2350–; doi:10.1021/cg400036x

data_4507799
_publ_section_title
;
 Two-Dimensional and Three-Dimensional Coordination Polymers of
 Hexakis(4-cyanophenyl)[3]radialene: The Role of Stoichiometry and
 Kinetics
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2350
_journal_paper_doi               10.1021/cg400036x
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C50 H30 Ag B F4 N8 O4'
_chemical_formula_weight         1001.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.269(7)
_cell_angle_beta                 98.944(5)
_cell_angle_gamma                102.439(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3749(6)
_cell_length_b                   15.3886(11)
_cell_length_c                   17.2299(11)
_cell_measurement_reflns_used    12890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2844
_cell_measurement_theta_min      2.6422
_cell_volume                     2167.6(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2003)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
  1 omega  -55.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463    0.0000   30.0000 113

  2 omega   -6.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   77.0000  150.0000 90

  3 omega  -51.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -77.0000   30.0000 101

  4 omega  -19.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   91.0000 -104.0000 25

  5 omega  -28.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -91.0000  -75.0000 36

  6 omega  -92.00  -42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  179.0000  150.0000 50

  7 omega  -34.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -91.0000  -75.0000 92

  8 omega  -98.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  179.0000 -120.0000 66

  9 omega  -33.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -91.0000  -75.0000 52

 10 omega  -98.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  179.0000   60.0000 66

 11 omega  -92.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -37.0000    0.0000 100

 12 omega  -19.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   91.0000 -104.0000 52

 13 omega  -13.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   77.0000   90.0000 66

 14 omega  -51.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276   77.0000   30.0000 102

 15 omega  -51.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276   77.0000  150.0000 102

;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48646
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'diamond-shaped block'
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         10494
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+4.6320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                7506
_reflns_number_total             10494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400036x_si_001.cif
_cod_data_source_block           2c
_cod_original_cell_volume        2167.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4507799