Azepiphthalocyanine—an unprecedented large twist of a π-conjugation system upon core-modification with a seven-membered ring unit
Shimizu, Soji; Zhu, Hua; Kobayashi, Nagao; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 3072–3072; doi:10.1039/c0cc05276k

data_7106079
_publ_section_title
;
 Azepiphthalocyanine---an unprecedented large twist of a \p-conjugation
 system upon core-modification with a seven-membered ring unit
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3072
_journal_page_last               3072
_journal_paper_doi               10.1039/c0cc05276k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C98 H92 N8 Ni, 3(C7 H8)'
_chemical_formula_sum            'C119 H116 N8 Ni'
_chemical_formula_weight         1716.91
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                90.0000(5)
_cell_angle_beta                 108.6367(5)
_cell_angle_gamma                90.0000(5)
_cell_formula_units_Z            4
_cell_length_a                   21.907(4)
_cell_length_b                   25.058(5)
_cell_length_c                   22.196(4)
_cell_measurement_reflns_used    19834
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.2689
_cell_measurement_theta_min      1.7764
_cell_volume                     11545(4)
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir 2004'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn70 CCD (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            140563
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         20299
_refine_ls_number_restraints     813
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0989
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+11.8667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2550
_refine_ls_wR_factor_ref         0.2695
_reflns_number_gt                17348
_reflns_number_total             20299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC05276K.TXT
_cod_data_source_block           091118
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

 Updated bibliographical information.

 Antanas Vaitkus,
 2019-09-23
;
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7106079