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_7705848
_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
'2(C33 H16 Ga N9), 2(C18 H36 K N2 O6), C6 H4 Cl2'
_chemical_formula_sum            'C108 H108 Cl2 Ga2 K2 N22 O12'
_chemical_formula_weight         2194.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-18
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5924)
;
_audit_update_record
;
2020-09-19 deposited with the CCDC.	2020-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 137.663(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.553(2)
_cell_length_b                   13.5280(2)
_cell_length_c                   28.9510(17)
_cell_measurement_reflns_used    15806
_cell_measurement_temperature    118.00(14)
_cell_measurement_theta_max      28.9420
_cell_measurement_theta_min      2.2840
_cell_volume                     9905(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      118.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.892
_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    -14.00  77.00   1.00  120.00    --   11.89  37.00  30.00   91
  2  \w    -20.00  72.00   1.00  120.00    --   11.89  77.00 120.00   92
  3  \w      6.00  32.00   1.00  120.00    --   11.89  77.00-150.00   26
  4  \w    -61.00  38.00   1.00  120.00    --   11.89 -37.00-150.00   99
;
_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      0.0134118000
_diffrn_orient_matrix_UB_12      0.0091004000
_diffrn_orient_matrix_UB_13      0.0339552000
_diffrn_orient_matrix_UB_21      -0.0246018000
_diffrn_orient_matrix_UB_22      0.0025609000
_diffrn_orient_matrix_UB_23      -0.0118909000
_diffrn_orient_matrix_UB_31      0.0011388000
_diffrn_orient_matrix_UB_32      -0.0515722000
_diffrn_orient_matrix_UB_33      0.0053890000
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            42022
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.371
_diffrn_reflns_theta_min         1.610
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.414
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.319(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1411
_refine_ls_number_reflns         18718
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0776P)^2^+10.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.540
_reflns_Friedel_fraction_full    0.647
_reflns_Friedel_fraction_max     0.482
_reflns_number_gt                16928
_reflns_number_total             18718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03404e2.cif
_cod_data_source_block           exp_848_int5
_cod_original_cell_volume        9905.5(16)
_cod_database_code               7705848
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C108 H108 Cl2 Ga2 K2 N22 O12'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.746
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.681(10)
 0.319(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C62 \\sim C52 \\sim C63 \\sim C64 \\sim C54 \\sim C65 \\sim C55 \\sim C66 \\sim
C56 \\sim C51 \\sim C61: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
Cl52 \\sim Cl62 \\sim Cl51 \\sim Cl61: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
Uanis(C66) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O32B) = Uanis(O32A)
4. Same fragment restrains
{Cl51, Cl52, C51, C52, C53, C54, C55, C56} sigma for 1-2: 0.001, 1-3: 0.001
as in
{Cl61, Cl62, C61, C62, C63, C64, C65, C66}
5. Others
 Sof(Cl61)=Sof(Cl62)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=1-FVAR(1)
 Sof(Cl51)=Sof(Cl52)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(1)
 Sof(H30I)=Sof(H30J)=Sof(H30M)=Sof(H30N)=Sof(O32B)=1-FVAR(2)
 Sof(O32A)=Sof(H30G)=Sof(H30H)=Sof(H30K)=Sof(H30L)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C304(H30I,
 H30J), C305(H30K,H30L), C305(H30M,H30N), C306(H30O,H30P), C307(H30Q,H30R),
 C308(H30S,H30T), C309(H30U,H30V), 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)
6.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105), C106(H106), C111(H111), C112(H112),
 C113(H113), C114(H114), C119(H119), C120(H120), C121(H121), C122(H122),
 C127(H127), C128(H128), C129(H129), C130(H130), C203(H203), C204(H204),
 C205(H205), C206(H206), C211(H211), C212(H212), C213(H213), C214(H214),
 C219(H219), C220(H220), C221(H221), C222(H222), C227(H227), C228(H228),
 C229(H229), C230(H230), C53(H53), C54(H54), C55(H55), C56(H56), C63(H63),
 C64(H64), C65(H65), C66(H66)
;
_shelx_res_checksum              45544
_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 1.093
_oxdiff_exptl_absorpt_empirical_full_min 0.915