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_7061257
_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, 4(F6 P)'
_chemical_formula_sum            'C117 H140 F24 Fe2 N10 O3 P8 Ru'
_chemical_formula_weight         2650.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc24rr1q
_audit_creation_date             2022-01-22
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.530(6)
_cell_length_b                   26.984(5)
_cell_length_c                   34.406(7)
_cell_measurement_reflns_used    69260
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.0012
_cell_volume                     26488(9)
_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)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0946
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            201480
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.047
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'RIGAKU/MSC(2004),CrystalClear Version 1.3.6'
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             10944
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.225
_refine_diff_density_max         1.753
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1360
_refine_ls_number_reflns         30180
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0841
_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^)+(0.1324P)^2^+29.1908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22648
_reflns_number_total             30180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05900a2.cif
_cod_data_source_block           c
_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_original_cell_volume        26487(9)
_cod_database_code               7061257
_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
 P6-F7 = P6-F8 = P6-F9 = P6-F10 = P6-F11 = P6-F12
 1.58 with sigma of 0.01
 F9-F10 = F8-F12 = F7-F11
 3.16 with sigma of 0.02
 F7-F10 = F7-F8 = F7-F9 = F7-F12 = F10-F8 = F10-F11 = F10-F12
 2.23 with sigma of 0.02
 F8-F11 = F8-F9
 2.23 with sigma of 0.02
 P6-F7A = P6-F8A = P6-F9A = P6-F10A = P6-F11A = P6-F12A
 1.58 with sigma of 0.01
 F7A-F10A = F8A-F11A = F9A-F12A
 3.16 with sigma of 0.02
 F7A-F11A = F7A-F9A = F7A-F8A = F7A-F12A = F11A-F9A = F11A-F10A
 2.23 with sigma of 0.02
 F11A-F12A = F9A-F10A = F9A-F8A
 2.23 with sigma of 0.02
 P5-F1A = P5-F2A = P5-F3A = P5-F4A = P5-F5 = P5-F6
 1.58 with sigma of 0.01
 F1A-F3A = F2A-F4A = F5-F6
 3.16 with sigma of 0.02
 F5-F1A = F5-F4A = F5-F3A = F5-F2A = F4A-F6 = F4A-F3A = F4A-F1A
 2.23 with sigma of 0.02
 F3A-F2A = F3A-F6
 2.23 with sigma of 0.02
3. Rigid bond restraints
 C57, C58, C54, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(F3) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F2) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 F7A, P6, F11, F8, F8A, F12A, F9, F11A, F9A, F10, F12, F10A, F7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) F1A(0.5) F2A(0.5) F3A(0.5)
 F4A(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) F7A(0.5) F8A(0.5)
 F9A(0.5) F10A(0.5) F11A(0.5) F12A(0.5)
7.a 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)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C75(H75A,H75B), C76(H76A,H76B)
7.c 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), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C)
7.d 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)
;
_shelx_res_checksum              33960
_shelx_fab_checksum              1655
_olex2_submission_special_instructions 'No special instructions were received'