Planar Ni(ii), Cu(ii) and Co(ii) tetraaza[14]annulenes: structural, electronic and magnetic properties and application to field effect transistors
Whyte, Alexander M.; Shuku, Yoshiaki; Nichol, Gary S.; Matsushita, Michio M.; Awaga, Kunio; Robertson, Neil; Journal of Materials Chemistry 22 (2012) 17967–; doi:10.1039/c2jm33079b

data_7238544
_publ_section_title
;
 Planar Ni(ii), Cu(ii) and Co(ii) tetraaza[14]annulenes: structural,
 electronic and magnetic properties and application to field effect
 transistors
;
_journal_issue                   34
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              17967
_journal_paper_doi               10.1039/c2jm33079b
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         '2(C18 H14 Cl Co N4), C7 H8'
_chemical_formula_sum            'C43 H36 Cl2 Co2 N8'
_chemical_formula_weight         853.58
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             11-04-27
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                74.895(7)
_cell_angle_beta                 81.155(7)
_cell_angle_gamma                75.541(8)
_cell_formula_units_Z            2
_cell_length_a                   9.3850(9)
_cell_length_b                   13.3040(12)
_cell_length_c                   15.3654(11)
_cell_measurement_reflns_used    11308
_cell_measurement_temperature    100
_cell_measurement_theta_max      73
_cell_measurement_theta_min      3
_cell_volume                     1785.5(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34656
_diffrn_reflns_theta_full        68.578
_diffrn_reflns_theta_max         72.955
_diffrn_reflns_theta_min         2.992
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.023
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.17
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1254
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.0023949
_refine_ls_shift/su_mean         0.0000942
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
43.6 42.2 43.2 22.4 3.99
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0767
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0728
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5964
_reflns_number_total             6975
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.65
_oxford_diffrn_Wilson_scale      0.10
_oxford_refine_ls_r_factor_ref   0.0833
_oxford_refine_ls_scale          3.633(11)
_oxford_reflns_number_all        6934
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'NR1003 in P-1'
_cod_data_source_file            c2jm33079b.txt
_cod_data_source_block           NR1003
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_hydrogens' value 'difmap,geom' was
changed to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7238544
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
SUMFIX ELEMENT SCALES
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) H ( 373,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 42,X'S) H ( 424,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
DIST 1.35 , 0.001 = C(37) TO C(40,-1,1,1,1)
DIST 1.35 , 0.001 = C(41) TO C(39,-1,1,1,1)
DIST 1.35 , 0.001 = C(41) TO C(41,-1,1,1,1)
DIST 1.35 , 0.001 = C(37) TO C(41)
DIST 1.35 , 0.001 = C(39) TO C(41)
DIST 1.35 , 0.001 = C(37) TO C(38)
DIST 1.35 , 0.001 = C(39) TO C(40)
ANGLE 120.000000 , 1.0000 = C(39) TO C(41) TO C(37)
ANGLE 120.000000 , 1.0000 = C(41) TO C(39) TO C(40)
ANGLE 120.000000 , 1.0000 = C(37) TO C(38) TO C(39)
ANGLE 120.000000 , 1.0000 = C(38) TO C(39) TO C(41,-1,1,1,1)
ANGLE 120.000000 , 1.0000 = C(39) TO C(41) TO C(39,-1,1,1,1)
ANGLE 180.000000 , 1.0000 = C(38) TO C(39) TO C(40)
U(IJ)'S 0.0, 0.01000 = C(38) TO C(40)
U(IJ)'S 0.0, 0.01000 = C(38) TO C(41)
U(IJ)'S 0.0, 0.010000 = C(39) TO C(37)
DIST 1.35 , 0.001 = C(37) TO C(40,-1,1,1,1)
DIST 1.35 , 0.001 = C(41) TO C(39,-1,1,1,1)
DIST 1.35 , 0.001 = C(41) TO C(41,-1,1,1,1)
DIST 1.35 , 0.001 = C(42) TO C(43)
DIST 1.35 , 0.001 = C(42) TO C(46)
DIST 1.35 , 0.001 = C(43) TO C(44)
DIST 1.35 , 0.001 = C(44) TO C(45)
DIST 1.35 , 0.001 = C(44) TO C(46)
ANGLE 120.000000 , 1.0000 = C(42) TO C(43) TO C(44)
ANGLE 120.000000 , 1.0000 = C(42) TO C(46) TO C(44)
ANGLE 120.000000 , 1.0000 = C(45) TO C(44) TO C(46)
ANGLE 120.000000 , 1.0000 = C(43) TO C(44) TO C(46,-1,1,2,0,1)
ANGLE 120.000000 , 1.0000 = C(44) TO C(46) TO C(44,-1,1,2,0,1)
ANGLE 180.000000 , 1.0000 = C(43) TO C(44) TO C(45)
U(IJ)'S 0.0, 0.010000 = C(46) TO C(45)
U(IJ)'S 0.0, 0.010000 = C(44) TO C(43)
U(IJ)'S 0.0, 0.010000 = C(42) TO C(45)
U(IJ)'S 0.0, 0.010000 = C(44) TO C(39)
U(IJ)'S 0.0, 0.010000 = C(46) TO C(41)
END
;