Trinuclear coordination assemblies of low-spin dicyano manganese(ii) (S = 1/2) and iron(ii) (S = 0) phthalocyanines with manganese(ii) acetylacetonate, tris(cyclopentadienyl)gadolinium(iii) and neodymium(iii)
Romanenko, Nikita R.; Kuzmin, Alexey V.; Mikhailenko, Maxim V.; Faraonov, Maxim A.; Khasanov, Salavat S.; Yudanova, Evgeniya I.; Shestakov, Alexander F.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01052F

data_7710494
_publ_section_title
;
 Trinuclear coordination assemblies of low-spin dicyano manganese(ii) (S =
 1/2) and iron(ii) (S = 0) phthalocyanines with manganese(ii)
 acetylacetonate, tris(cyclopentadienyl)gadolinium(iii) and neodymium(iii)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01052F
_journal_year                    2022
_chemical_formula_moiety
'C64 H46 Gd2 Mn N10, 2(C18 H36 K N2 O6), 4(C6 H4 Cl2)'
_chemical_formula_sum            'C124 H134 Cl8 Gd2 K2 Mn N14 O12'
_chemical_formula_weight         2743.68
_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             2021-10-23
_audit_creation_method
;
FinalCif V89 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-10-23 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                73.112(2)
_cell_angle_beta                 78.193(2)
_cell_angle_gamma                67.321(2)
_cell_formula_units_Z            1
_cell_length_a                   13.9492(3)
_cell_length_b                   14.2598(2)
_cell_length_c                   17.5018(3)
_cell_measurement_reflns_used    1600
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.0
_cell_volume                     3056.67(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      106(2)
_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_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_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     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36115
_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         26.000
_diffrn_reflns_theta_min         1.865
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.483
_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    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1399
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         12027
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+3.9460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11622
_reflns_number_total             12027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01052f2.cif
_cod_data_source_block           shelx
_cod_database_code               7710494
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.756
_shelx_estimated_absorpt_t_max   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C64 \\sim C65 \\sim C66 \\sim C61 \\sim C62 \\sim C63: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
3. 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}
4. 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)
5.a Free rotating group:
 Cl51(Cl52,C51,C52,C53,C54,C55,C56)
5.b 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)
5.c Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C106(H106), C107(H107), C112(H112), C113(H113),
 C114(H114), C115(H115), C201(H201), C202(H202), C203(H203), C204(H204),
 C205(H205), C206(H206), C207(H207), C208(H208), C209(H209), C210(H210),
 C211(H211), C212(H212), C213(H213), C214(H214), C215(H215), C43(H43), C44(H44),
  C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56), C63(H63),
 C64(H64), C65(H65), C66(H66)
;