1,4,8,11,15,18,22,25-Alkylsulfanyl phthalocyanines: effect of macrocycle distortion on spectroscopic and packing properties
Yunus Zorlu; Ufuk Kumru; Umit Isci; Burcin Divrik; Erwann Jeanneau; Florian Albrieux; Yavuz Dede; Vefa Ahsen; Fabienne Dumoulin; Chem.Commun. 51 (2015) 6580–; doi:10.1039/C5cc01085C

data_7116907
_publ_section_title
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 1,4,8,11,15,18,22,25-Alkylsulfanyl phthalocyanines: effect of macrocycle
 distortion on spectroscopic and packing properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              6580
_journal_paper_doi               10.1039/C5cc01085C
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C64 H82 N8 S8 '
_chemical_formula_sum            'C64 H82 N8 S8'
_chemical_formula_weight         1219.94
_space_group_IT_number           218
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2015-02-01 deposited with the CCDC.
2015-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   22.6217(4)
_cell_length_b                   22.6217(4)
_cell_length_c                   22.6217(4)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    120
_cell_measurement_theta_max      16.7037
_cell_measurement_theta_min      1.7985
_cell_volume                     11576.5(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            4450
_diffrn_reflns_theta_full        27.517
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         1.273
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.8984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3900
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.380
_platon_squeeze_details
;
;
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.43
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.032(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0092
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.0006176
_refine_ls_shift/su_mean         0.0000439
_refine_ls_structure_factor_coef Fsqd
_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: 
 12.7 19.8 9.66 2.44 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1917
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1917
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              1
_reflns_number_gt                3464
_reflns_number_total             4450
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.09
_oxford_diffrn_Wilson_scale      191.98
_oxford_refine_ls_r_factor_ref   0.0803
_oxford_refine_ls_scale          0.07304(4)
_oxford_reflns_number_all        4450
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c5cc01085c2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     'P -4n 2 3 '
_cod_original_sg_symbol_H-M      'P -4 3 n '
_cod_original_formula_sum        'C64 H82 N8 S8 '
_cod_database_code               7116907
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  83,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  91,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 103,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE N   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  18,X'S) H   ( 183,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 202,X'S) H   ( 201,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.0020000 = C(8) TO C(7) 
U(IJ)'S  0.0, 0.0020000 = C(9) TO C(7) 
U(IJ)'S  0.0, 0.0020000 = C(10) TO C(7) 
VIBRATION 0.0, 0.010000 = S(6) TO C(7) 
END                                                                             
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