Molecular structure, optical and magnetic properties of free-base tetrapyrazinoporphyrazine in various reduction states
Konarev, Dmitri V.; Faraonov, Maxim A.; Kuz`min, Alexey V.; Osipov, Nikita G.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; New Journal of Chemistry 43 (2019) 19214–19222; doi:10.1039/C9NJ04775A

data_7059048
_publ_section_title
;
 Molecular structure, optical and magnetic properties of free-base
 tetrapyrazinoporphyrazine in various reduction states
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19214
_journal_page_last               19222
_journal_paper_doi               10.1039/C9NJ04775A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C6 H4 Cl2, 2(C18 H36 K N2 O6), 2(C12 H5 N8)'
_chemical_formula_sum            'C66 H86 Cl2 K2 N20 O12'
_chemical_formula_weight         1500.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-08 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.290(4)
_cell_angle_beta                 99.291(3)
_cell_angle_gamma                95.730(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8535(3)
_cell_length_b                   15.7516(7)
_cell_length_c                   24.2437(11)
_cell_measurement_reflns_used    6167
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      25.6610
_cell_measurement_theta_min      1.7600
_cell_volume                     3593.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.828
_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      1.00  40.00   1.00   96.00    --   11.89 -99.00-120.00   39
  2  \w   -102.00 -66.00   1.00   96.00    --  -12.20-178.00   0.00   36
  3  \w      9.00  61.00   1.00   96.00    --  -12.20  37.00  90.00   52
  4  \w     -3.00  36.00   1.00   96.00    --  -12.20-124.00 154.00   39
  5  \w    -13.00  28.00   1.00   96.00    --  -12.20 -99.00-150.00   41
  6  \w    -88.00  23.00   1.00   96.00    --  -12.20 -19.00 -60.00  111
  7  \w    -38.00  -9.00   1.00   96.00    --  -12.20  37.00   0.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0132411000
_diffrn_orient_matrix_UB_12      0.0007385000
_diffrn_orient_matrix_UB_13      -0.0295218000
_diffrn_orient_matrix_UB_21      0.0187627000
_diffrn_orient_matrix_UB_22      -0.0427353000
_diffrn_orient_matrix_UB_23      -0.0072258000
_diffrn_orient_matrix_UB_31      -0.0699867000
_diffrn_orient_matrix_UB_32      -0.0184138000
_diffrn_orient_matrix_UB_33      -0.0023812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.1320
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34558
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.667
_diffrn_reflns_theta_min         1.751
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.687
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         16824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0177P)^2^+5.6375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8843
_reflns_number_total             16824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04775a2.cif
_cod_data_source_block           exp_1312_int1
_cod_database_code               7059048
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H66N18Cl2K1V2
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C109(H10Q,H10R),
 C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C114(H11I,
 H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P), C118(H11Q,H11R),
 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), C215(H21K,H21L), C216(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C54(H54), C55(H55), C56(H56), C304(H304), C305(H305), C310(H310),
 C311(H311), N301(H301), C404(H404), C405(H405), C410(H410), C411(H411),
 N401(H401)
;
_shelx_res_checksum              20092
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.840