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_7705849
_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         'C65 H64 K N9 O6 Sn'
_chemical_formula_sum            'C65 H64 K N9 O6 Sn'
_chemical_formula_weight         1225.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-11
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_audit_update_record
;
2020-09-19 deposited with the CCDC.	2020-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.490(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0694(3)
_cell_length_b                   23.4397(6)
_cell_length_c                   18.9431(4)
_cell_measurement_reflns_used    11835
_cell_measurement_temperature    124(7)
_cell_measurement_theta_max      31.0000
_cell_measurement_theta_min      2.1390
_cell_volume                     5785.3(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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      124(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -6.00  96.00   1.00  100.00    --   20.30  37.00 -30.00  102
  2  \w    -25.00   0.00   1.00  100.00    --  -20.45 -99.00-180.00   25
  3  \w    -39.00  48.00   1.00  100.00    --  -20.45  57.00 150.00   87
  4  \w    -16.00  18.00   1.00  100.00    --  -20.45 -99.00 -90.00   34
;
_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      0.0508408000
_diffrn_orient_matrix_UB_12      -0.0098756000
_diffrn_orient_matrix_UB_13      0.0083788000
_diffrn_orient_matrix_UB_21      -0.0179220000
_diffrn_orient_matrix_UB_22      -0.0285767000
_diffrn_orient_matrix_UB_23      -0.0009261000
_diffrn_orient_matrix_UB_31      0.0077312000
_diffrn_orient_matrix_UB_32      -0.0015319000
_diffrn_orient_matrix_UB_33      -0.0365699000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30885
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96505
_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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane by solvent layering'
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         11367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0264P)^2^+2.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9137
_reflns_number_total             11367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03404e2.cif
_cod_data_source_block           exp_1247_int1
_cod_database_code               7705849
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.809
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.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), C215(H21K,H21L), C216(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C119(H119), C120(H120), C121(H121),
 C122(H122), C123(H123), C125(H125), C126(H126), C130(H130), C131(H131),
 C132(H132), C133(H133), C134(H134), C136(H136), C137(H137), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144)
;
_shelx_res_checksum              18115
_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 1.072
_oxdiff_exptl_absorpt_empirical_full_min 0.915