Reaction of Ga<sup>III</sup>ClPc, Sn<sup>IV</sup>Cl<sub>2</sub>TPP and B<sup>III</sup>ClSubPc with cyanide anions: reduction of macrocycles <i>vs.</i> formation of cyano-containing macrocyclic anions.
Konarev, Dmitri V.; Kuzmin, Alexey V.; Shestakov, Alexander F.; Rompanen, Ivan A.; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16801–16812; doi:10.1039/d0dt03404e

data_7705850
_publ_section_title
;
 Reaction of Ga<sup>III</sup>ClPc, Sn<sup>IV</sup>Cl<sub>2</sub>TPP and
 B<sup>III</sup>ClSubPc with cyanide anions: reduction of macrocycles
 <i>vs.</i> formation of cyano-containing macrocyclic anions.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16801
_journal_page_last               16812
_journal_paper_doi               10.1039/d0dt03404e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C18 H35 K N2 O6, C18 H34 K N2 O6, 2(C6 H4 Cl2), C54 H24 B2 N18, 1[C6H4Cl2]'
_chemical_formula_sum            'C108 H114 B2 Cl6 K2 N22 O12'
_chemical_formula_weight         2224.73
_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             2020-09-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-19 deposited with the CCDC.	2020-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.018(2)
_cell_angle_beta                 91.803(2)
_cell_angle_gamma                104.868(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4390(2)
_cell_length_b                   15.2417(3)
_cell_length_c                   25.1736(6)
_cell_measurement_reflns_used    29492
_cell_measurement_temperature    124(7)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      1.9470
_cell_volume                     5303.07(19)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      124(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_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     38.00 102.00   1.00   50.00    --   11.89 178.00 -60.00   64
  2  \w     38.00  74.00   1.00   50.00    --   11.89-132.00 114.00   36
  3  \w    -82.00  69.00   1.00   50.00    --  -12.20   0.00 150.00  151
  4  \w    -83.00  14.00   1.00   50.00    --  -12.20 -37.00 -30.00   97
  5  \w    -25.00  30.00   1.00   50.00    --  -12.20 -99.00-120.00   55
  6  \w    -74.00 -22.00   1.00   50.00    --  -12.20 132.00-123.41   52
  7  \w    -94.00  34.00   1.00   50.00    --  -12.20 -19.00  60.00  128
  8  \w    -73.00 -33.00   1.00   50.00    --  -12.20 130.00 148.35   40
;
_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      -0.0098693000
_diffrn_orient_matrix_UB_12      -0.0301393000
_diffrn_orient_matrix_UB_13      -0.0244909000
_diffrn_orient_matrix_UB_21      -0.0116052000
_diffrn_orient_matrix_UB_22      -0.0380720000
_diffrn_orient_matrix_UB_23      0.0144712000
_diffrn_orient_matrix_UB_31      -0.0486034000
_diffrn_orient_matrix_UB_32      0.0018411000
_diffrn_orient_matrix_UB_33      -0.0004345000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            92838
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.686
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99662
_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    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             2324
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane by solvent layering'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1316
_refine_ls_number_reflns         26413
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1322P)^2^+7.4613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.2494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18531
_reflns_number_total             26413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03404e2.cif
_cod_data_source_block           exp_1252_int1
_cod_database_code               7705850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.912
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 C12A-C101 \\sim C102-C101
 with sigma of 0.02
 C107-C102 \\sim C17A-C12A
 with sigma of 0.02
 C108-C107 \\sim C17A-C108
 with sigma of 0.02
 C103-C102 \\sim C13A-C12A
 with sigma of 0.02
 C14A-C13A \\sim C104-C103
 with sigma of 0.02
 C105-C104 \\sim C15A-C14A
 with sigma of 0.02
 C16A-C15A \\sim C106-C105
 with sigma of 0.02
 C107-C106 \\sim C17A-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) = Uanis(C102)
Uanis(C13A) = Uanis(C103)
Uanis(C14A) = Uanis(C104)
Uanis(C15A) = Uanis(C105)
Uanis(C106) = Uanis(C16A)
Uanis(C17A) = Uanis(C107)
4. Others
 Sof(C17A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=
 Sof(C13A)=Sof(H13A)=Sof(C12A)=1-FVAR(1)
 Sof(C102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(H10A)=Sof(C105)=Sof(H105)=
 Sof(C106)=Sof(H10B)=Sof(C107)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C307(H30M,H30N), C308(H30O,H30P), C309(H30Q,H30R),
 C310(H31A,H31B), C311(H31C,H31D), C312(H31E,H31F), C313(H31G,H31H), C314(H31I,
 H31J), C315(H31K,H31L), C316(H31M,H31N), C317(H31O,H31P), C318(H31Q,H31R),
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C404(H40G,H40H), C405(H40I,
 H40J), C406(H40K,H40L), C407(H40M,H40N), C408(H40O,H40P), C409(H40Q,H40R),
 C410(H41A,H41B), C411(H41C,H41D), C412(H41E,H41F), C413(H41G,H41H), C414(H41I,
 H41J), C415(H41K,H41L), C416(H41M,H41N), C417(H41O,H41P), C418(H41Q,H41R)
5.b Aromatic/amide H refined with riding coordinates:
 N102(H102), N104(H104), N106(H106), N202(H202), N204(H204), N206(H206),
 C53(H53), C54(H54), C55(H55), C56(H56), C63(H63), C64(H64), C65(H65), C66(H66),
  C103(H103), C104(H10A), C105(H105), C106(H10B), C111(H111), C112(H112),
 C113(H113), C114(H114), C119(H119), C120(H120), C121(H121), C122(H122),
 C203(H203), C204(H20A), C205(H205), C206(H20B), C211(H211), C212(H212),
 C213(H213), C214(H214), C219(H219), C220(H220), C221(H221), C222(H222),
 C16A(H16A), C15A(H15A), C14A(H14A), C13A(H13A)
;
_smtbx_masks_void_probe_radius   1.5
_smtbx_masks_void_truncation_radius 1.3
_shelx_res_checksum              56095
_shelx_fab_checksum              54570
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_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 1.034
_oxdiff_exptl_absorpt_empirical_full_min 0.972