Effect of reduction on the molecular structure and optical and magnetic properties of fluorinated copper(II) phthalocyanines.
Konarev, Dmitri V.; Faraonov, Maxim A.; Batov, Mikhail S.; Andronov, Mikhail G.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16821–16829; doi:10.1039/d0dt02635b

data_7705702
_publ_section_title
;
 Effect of reduction on the molecular structure and optical and magnetic
 properties of fluorinated copper(II) phthalocyanines.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16821
_journal_page_last               16829
_journal_paper_doi               10.1039/d0dt02635b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 Cu F16 N8, 2(C18 H36 N2 Na O6)'
_chemical_formula_sum            'C68 H72 Cu F16 N12 Na2 O12'
_chemical_formula_weight         1662.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-23
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-23 deposited with the CCDC.	2020-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.615(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0273(5)
_cell_length_b                   11.7156(2)
_cell_length_c                   30.5920(7)
_cell_measurement_reflns_used    17335
_cell_measurement_temperature    117.6(9)
_cell_measurement_theta_max      29.1160
_cell_measurement_theta_min      3.7280
_cell_volume                     7481.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      118
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  71.00   1.00   80.00    --   11.89  37.00 120.00   83
  2  \w      9.00  85.00   1.00   80.00    --   11.89  37.00 -30.00   76
  3  \w     10.00  93.00   1.00   80.00    --   11.89  19.00  30.00   83
  4  \w    -25.00  30.00   1.00   80.00    --  -12.05 -99.00 -90.00   55
  5  \w    -25.00   2.00   1.00   80.00    --  -12.05 -99.00-150.00   27
  6  \w    -25.00   0.00   1.00   80.00    --  -12.05 -99.00 150.00   25
  7  \w     17.00  60.00   1.00   80.00    --  -12.05  37.00-150.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            39693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.875
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             3420
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+7.9284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6583
_reflns_number_total             8927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02635b2.cif
_cod_data_source_block           exp_824
_cod_depositor_comments
'Adding full bibliography for 7705702--7705703.cif.'
_cod_database_code               7705702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Na21-O25A \\sim Na21-O25B
 with sigma of 0.02
 O26A-C25A \\sim O26B-C25B
 with sigma of 0.04
 Na21-O26A \\sim Na21-O26B
 with sigma of 0.02
 C26A-C217 \\sim C26B-C217
 with sigma of 0.04
 O25A-C214 \\sim O25B-C214
 with sigma of 0.02
 O25A-C25A \\sim O25B-C25B
 with sigma of 0.02
 O26A-C26A \\sim O26B-C26B
 with sigma of 0.02
 O26A-C217 \\sim O26B-C217
 with sigma of 0.02
 C214-C25A \\sim C214-C25B
 with sigma of 0.04
 C25A-C26A \\sim C25B-C26B
 with sigma of 0.02
 Na21-C25A \\sim Na21-C25B
 with sigma of 0.04
 Na21-C26A \\sim Na21-C26B
 with sigma of 0.04
 O25A-C26A \\sim O25B-C26B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C25B) = Uanis(C25A)
Uanis(O26B) = Uanis(O26A)
Uanis(O25B) = Uanis(O25A)
Uanis(C26B) = Uanis(C26A)
4. Others
 Sof(H21K)=Sof(H21L)=Sof(H21O)=Sof(H21P)=Sof(O25B)=Sof(O26B)=Sof(C25B)=
 Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=1-FVAR(1)
 Sof(H21I)=Sof(H21J)=Sof(H21M)=Sof(H21N)=Sof(O25A)=Sof(O26A)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C208(H20O,H20P), C209(H20Q,H20R),
 C210(H21A,H21B), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J), C214(H21K,H21L), C217(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R),
 C25A(H25A,H25B), C26A(H26A,H26B), C25B(H25C,H25D), C26B(H26C,H26D)
;
_shelx_res_checksum              45122
_shelx_fab_checksum              32477
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;