Temperature-resolved study of the structural behaviour of nickel octahexyl phthalocyanine up to the liquid crystal transition
Helliwell, Madeleine; Teat, Simon J.; Coles, Simon J.; Reeve, William; Acta Crystallographica Section B 59 (2003) 617–624; doi:10.1107/S0108768103014708

data_2103952
_publ_section_title
;
 Temperature-resolved study of the structural behaviour of nickel
 octahexyl phthalocyanine up to the liquid crystal transition
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              617
_journal_page_last               624
_journal_paper_doi               10.1107/S0108768103014708
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C80 H112 N8 Ni'
_chemical_formula_sum            'C80 H112 N8 Ni'
_chemical_formula_weight         1244.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.518(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.468(3)
_cell_length_b                   37.010(7)
_cell_length_c                   18.942(3)
_cell_measurement_reflns_used    10082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      1.56
_cell_volume                     14331(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6874
_diffrn_reflns_av_R_equivalents  0.109
_diffrn_reflns_av_sigmaI/netI    0.166
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44174
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.50
_refine_ls_extinction_coef       0.00022(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.90
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         15611
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.91
_refine_ls_R_factor_all          0.218
_refine_ls_R_factor_gt           0.0751
_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^)+(0.0914P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.155
_refine_ls_wR_factor_ref         0.210
_reflns_number_gt                5808
_reflns_number_total             15611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5000.cif
_cod_data_source_block           293
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_database_code               2103952