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_7710492
_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         'C70 H72 Cl16 Fe K2 N14 O12, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C82 H80 Cl20 Fe K2 N14 O12'
_chemical_formula_weight         2296.65
_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             2021-10-21
_audit_creation_method
;
FinalCif V89 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-10-22 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.18320(10)
_cell_length_b                   19.5040(2)
_cell_length_c                   19.3262(2)
_cell_measurement_reflns_used    26991
_cell_measurement_temperature    111(8)
_cell_measurement_theta_max      29.4440
_cell_measurement_theta_min      1.8900
_cell_volume                     4859.87(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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      111(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.885
_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    -18.00  31.00   1.00  120.00    --   11.89  57.00  60.00   49
  2  \w     48.00  76.00   1.00  120.00    --   11.89  57.00  60.00   28
  3  \w    -30.00  -4.00   1.00  120.00    --  -12.20 -57.00-150.00   26
  4  \w    -48.00  12.00   1.00  120.00    --  -12.20 -57.00 -30.00   60
  5  \w    -78.00   9.00   1.00  120.00    --  -12.20 -57.00 120.00   87
  6  \w     -4.00  45.00   1.00  120.00    --  -12.20  57.00-180.00   49
  7  \w    -37.00  60.00   1.00  120.00    --  -12.20  57.00 -90.00   97
;
_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      0.0282768000
_diffrn_orient_matrix_UB_12      -0.0138514000
_diffrn_orient_matrix_UB_13      0.0322224000
_diffrn_orient_matrix_UB_21      0.0074436000
_diffrn_orient_matrix_UB_22      0.0334778000
_diffrn_orient_matrix_UB_23      0.0145215000
_diffrn_orient_matrix_UB_31      -0.0465943000
_diffrn_orient_matrix_UB_32      -0.0030661000
_diffrn_orient_matrix_UB_33      0.0126414000
_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  0.0211
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.690
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
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    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         12195
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0340P)^2^+3.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10260
_reflns_number_total             12195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01052f2.cif
_cod_data_source_block           exp_1361_int1
_cod_database_code               7710492
_chemical_oxdiff_formula         'C242  H220  N22  O22  '
_shelx_shelxl_version_number     2018/3
_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 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.894
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.904
_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
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C41 \\sim C42 \\sim
C43 \\sim C44 \\sim C45 \\sim C46: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(C31) \\sim Ueq, Uanis(Cl31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(Cl32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(Cl41) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(Cl42) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, : with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Same fragment restrains
{Cl31, Cl32, C31, C32, C33, C34, C35, C36} sigma for 1-2: 0.001, 1-3: 0.001
as in
{Cl41, Cl42, C41, C42, C43, C44, C45, C46}
4. Others
 Sof(Cl41)=Sof(Cl42)=Sof(C41)=Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=
 Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=1-FVAR(1)
 Sof(Cl31)=Sof(Cl32)=Sof(C31)=Sof(C32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=
 Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
5.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)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C35(H35), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46)
;