The syntheses, crystal structures, electrochemical and magnetic properties of tri-nuclear cyanide-bridged complexes [cis-MII(bpy)2(CN)2]2MnIII(salcy) (PF6) (M = Fe, Ru, Os)
Liu, Ming; Hu, Jianmei; Yu, Meng; Fan, Weiwei; Ding, Wenwen; Wang, Yong; New Journal of Chemistry 43 (2019) 3162–; doi:10.1039/C8NJ04142C

data_7058111
_publ_section_title
;
 The syntheses, crystal structures, electrochemical and magnetic
 properties of tri-nuclear cyanide-bridged complexes
 [cis-MII(bpy)2(CN)2]2MnIII(salcy) (PF6) (M = Fe, Ru, Os)
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3162
_journal_paper_doi               10.1039/C8NJ04142C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C64 H52 Fe2 Mn N14 O2, F6 P'
_chemical_formula_sum            'C64 H52 F6 Fe2 Mn N14 O2 P'
_chemical_formula_weight         1360.80
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-12-19 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.679(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.566(12)
_cell_length_b                   23.082(17)
_cell_length_c                   22.534(18)
_cell_measurement_reflns_used    19559
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.0306
_cell_volume                     7832(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2016/4)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2016/4)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2016/4)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42189
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5970
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.109
_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     871
_refine_ls_number_reflns         13329
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.1110
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3087
_refine_ls_wR_factor_ref         0.3336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8113
_reflns_number_total             13329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04142c2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7058109--7058111.cif.'
_cod_database_code               7058111
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C97-C95
 1.66 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C98 \\sim C97 \\sim N96 \\sim C101 \\sim C100 \\sim C99 \\sim C95 \\sim C94
\\sim C93 \\sim C92 \\sim C91 \\sim N90: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C23 \\sim O1 \\sim C29:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
N51 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim N40 \\sim C45 \\sim
C44 \\sim C43 \\sim C42 \\sim C41: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C97) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: N90(0.5) C95(0.5) C94(0.5) H94(0.5) C93(0.5) H93(0.5) C92(0.5)
 H92(0.5) C91(0.5) H91(0.5) C97(0.5) N96(0.5) C101(0.5) H101(0.5) C100(0.5)
 H100(0.5) C99(0.5) H99(0.5) C98(0.5) H98(0.5) C49(0.5) H49(0.5) C50(0.5)
 H50(0.5) N51(0.5) C46(0.5) C47(0.5) H47(0.5) C48(0.5) H48(0.5) C41(0.5)
 H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5)
 N40(0.5)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C54(H54)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C53(H53), C38(H38), C39(H39),
  C40(H40), C73(H73), C71(H71), C70(H70), C69(H69), C68(H68), C51(H51),
 C57(H57), C56(H56), C55(H55), C7AA(H7AA), C58(H58), C59(H59), C60(H60),
 C63(H63), C64(H64), C65(H65), C66(H66), C94(H94), C93(H93), C92(H92), C91(H91),
  C101(H101), C100(H100), C99(H99), C98(H98), C49(H49), C50(H50), C47(H47),
 C48(H48), C41(H41), C42(H42), C43(H43), C44(H44)
5.d Fitted hexagon refined as free rotating group:
 N90(C95,C94,C93,C92,C91), C97(N96,C101,C100,C99,C98), C49(C50,N51,C46,C47,
 C48), C41(C42,C43,C44,C45,N40)
;
_olex2_submission_special_instructions 'No special instructions were received'