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_7059049
_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
'2(C12 H5 N8), 2(C18 H36 K N2 O6), C14 H10 Cr2 O4, 3(C6 H4 Cl2)'
_chemical_formula_sum            'C92 H104 Cl6 Fe2 K2 N20 O16'
_chemical_formula_weight         2148.55
_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             2019-07-20
_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                108.314(2)
_cell_angle_beta                 94.677(2)
_cell_angle_gamma                110.394(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2775(3)
_cell_length_b                   18.5439(5)
_cell_length_c                   23.0154(5)
_cell_measurement_reflns_used    21371
_cell_measurement_temperature    115(6)
_cell_measurement_theta_max      29.2590
_cell_measurement_theta_min      1.7570
_cell_volume                     4925.0(2)
_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      115(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.841
_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     28.00  54.00   1.00   36.00    --   12.05 -99.00 150.00   26
  2  \w    -54.00  -2.00   1.00   36.00    --  -12.36  99.00 -31.00   52
  3  \w    -23.00  24.00   1.00   36.00    --  -12.36 -99.00-138.00   47
  4  \w    -37.00  69.00   1.00   36.00    --  -12.36  19.00-180.00  106
  5  \w    -39.00  59.00   1.00   36.00    --  -12.36  37.00  90.00   98
  6  \w     18.00  57.00   1.00   36.00    --  -12.36  57.00 150.00   39
  7  \w    -98.00 -59.00   1.00   36.00    --  -12.36-178.00  90.00   39
;
_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      -0.0126429000
_diffrn_orient_matrix_UB_12      -0.0390283000
_diffrn_orient_matrix_UB_13      0.0028410000
_diffrn_orient_matrix_UB_21      -0.0306000000
_diffrn_orient_matrix_UB_22      -0.0199319000
_diffrn_orient_matrix_UB_23      -0.0313832000
_diffrn_orient_matrix_UB_31      0.0480526000
_diffrn_orient_matrix_UB_32      -0.0019001000
_diffrn_orient_matrix_UB_33      -0.0105720000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55588
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.719
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90717
_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    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.574
_exptl_crystal_size_mid          0.397
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         23542
_refine_ls_number_restraints     498
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0530P)^2^+3.3108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18062
_reflns_number_total             23542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04775a2.cif
_cod_data_source_block           exp_1323_int1
_cod_database_code               7059049
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.89
_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 C(H,H,H,H) groups, All N(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.003
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.5A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(C49B)=Sof(H49B)=Sof(C48B)=Sof(H48B)=Sof(C47B)=Sof(H47B)=Sof(C46B)=
 Sof(H46B)=Sof(C50B)=Sof(H50B)=1-FVAR(1)
 Sof(C49A)=Sof(H49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=Sof(C46A)=
 Sof(H46A)=Sof(C50A)=Sof(H50A)=FVAR(1)
 Sof(C45B)=Sof(H45B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=
 Sof(H43B)=Sof(C44B)=Sof(H44B)=1-FVAR(2)
 Sof(C43A)=Sof(H43A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=Sof(C45A)=
 Sof(H45A)=Sof(C44A)=Sof(H44A)=FVAR(2)
 Sof(H21K)=Sof(H21L)=Sof(H21O)=Sof(H21P)=Sof(C25B)=Sof(H25C)=Sof(H25D)=
 Sof(O25B)=1-FVAR(3)
 Sof(H21I)=Sof(H21J)=Sof(H21M)=Sof(H21N)=Sof(C25A)=Sof(H25A)=Sof(H25B)=
 Sof(O25A)=FVAR(3)
5.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(H21K,
 H21L), C214(H21I,H21J), C216(H21O,H21P), C216(H21M,H21N), C217(H21Q,H21R),
 C218(H21S,H21T), C25A(H25A,H25B), C25B(H25C,H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C3AA(H3AA), C409(H409), C410(H410), N405(H405), C303(H303),
 C304(H304), C309(H309), C310(H310), N305(H305), C43A(H43A), C42A(H42A),
 C41A(H41A), C45A(H45A), C44A(H44A), C49A(H49A), C48A(H48A), C47A(H47A),
 C46A(H46A), C50A(H50A), C45B(H45B), C41B(H41B), C42B(H42B), C43B(H43B),
 C44B(H44B), C49B(H49B), C48B(H48B), C47B(H47B), C46B(H46B), C50B(H50B)
5.c Fitted pentagon refined as free rotating group:
 C43A(C42A,C41A,C45A,C44A), C49A(C48A,C47A,C46A,C50A), C45B(C41B,C42B,C43B,
 C44B), C49B(C48B,C47B,C46B,C50B)
;
_shelx_res_checksum              53538
_shelx_fab_checksum              2523
_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 1.144
_oxdiff_exptl_absorpt_empirical_full_min 0.848