Synthesis, structural and metal-to-metal charge transfer properties of cyanide-bridged compound [FeII/III-NC-RuII-CN-FeII/III]
Wang, Yong; New Journal of Chemistry 46 (2022) 3978–3984; doi:10.1039/D1NJ05900A

data_7061256
_publ_section_title
;
 Synthesis, structural and metal-to-metal charge transfer properties of
 cyanide-bridged compound [FeII/III-NC-RuII-CN-FeII/III]
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3978
_journal_page_last               3984
_journal_paper_doi               10.1039/D1NJ05900A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C100 H110 Fe2 N6 P4 Ru, 2(F6 P)'
_chemical_formula_sum            'C104 H118 Cl8 F12 Fe2 N6 P6 Ru'
_chemical_formula_weight         2362.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc24rr0p
_audit_creation_date             2022-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-25 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.100(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.838(3)
_cell_length_b                   30.951(8)
_cell_length_c                   25.870(7)
_cell_measurement_reflns_used    34554
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.1905
_cell_volume                     11017(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2016)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2016)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            77510
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.152
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'RIGAKU/MSC(2004),CrystalClear Version 1.3.6'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       prism
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         19340
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0596P)^2^+9.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15351
_reflns_number_total             19340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05900a2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061254--7061257.cif.
;
_cod_database_code               7061256
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C54-C57 \\sim C54-C57A
 with sigma of 0.02
 C57-C58 \\sim C57A-C58A
 with sigma of 0.02
 C63-C67 \\sim C63-C67A
 with sigma of 0.04
 C57-C59 \\sim C57A-C59A
 with sigma of 0.02
 C57-C60 \\sim C57A-C60A
 with sigma of 0.02
 C67-C69 \\sim C67A-C69A
 with sigma of 0.04
 C66-C69 \\sim C66A-C69A
 with sigma of 0.02
 C66-C67 \\sim C66A-C67A
 with sigma of 0.02
 C63-C69 \\sim C63-C69A
 with sigma of 0.04
 C54-C58 \\sim C54-C58A
 with sigma of 0.04
 C54-C59 \\sim C54-C59A
 with sigma of 0.04
 C54-C60 \\sim C54-C60A
 with sigma of 0.04
 C63-C66 \\sim C63-C66A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.04
 C66-C68 \\sim C66A-C68A
 with sigma of 0.02
 C58-C60 \\sim C58A-C60A
 with sigma of 0.04
 C63-C68 \\sim C63-C68A
 with sigma of 0.04
 C67-C68 \\sim C67A-C68A
 with sigma of 0.04
 C59-C60 \\sim C59A-C60A
 with sigma of 0.04
 C68-C69 \\sim C68A-C69A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C57A, C59A, C58A, C60A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C66, C67, C68, C69
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59D)=
 Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Sof(C66A)=Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C68A)=Sof(H68D)=
 Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=1-FVAR(2)
 Sof(C66)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(H68A)=Sof(H68B)=
 Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=FVAR(2)
 Fixed Uiso: C57A(0.06) C58A(0.06) C59A(0.06) C60A(0.06) C66A(0.06) C67A(0.06)
 C68A(0.06) C69A(0.06)
5.a Riding coordinates:
 C58A(H58D,H58E,H58F), C69A(H69D,H69E,H69F)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C70(H70), C71(H71), C72(H72),
 C73(H73), C74(H74)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C75(H75A,H75B), C76(H76A,H76B)
5.d Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C)
5.e Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C43(H43), C44(H44), C46(H46), C47(H47), C52(H52), C53(H53),
  C55(H55), C56(H56), C61(H61), C62(H62), C64(H64), C65(H65), C78(H78),
 C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87),
  C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100)
5.f Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C59A(H59D,H59E,H59F),
 C60A(H60D,H60E,H60F), C67A(H67D,H67E,H67F), C68A(H68D,H68E,H68F)
;
_shelx_res_checksum              78018
_shelx_fab_checksum              68227
_olex2_submission_special_instructions 'No special instructions were received'