Synthesis and structural and spectroscopic properties of a cyanido-bridged mixed-valence compound [Fe–NC–Ru–CN–Fe]
Liu, Ming; Xiong, Yan; Xu, Weixiu; Wang, Yong; New Journal of Chemistry 47 (2023) 6796–6803; doi:10.1039/D3NJ00049D

data_7062347
_publ_section_title
;
 Synthesis and structural and spectroscopic properties of a
 cyanido-bridged mixed-valence compound [Fe--NC--Ru--CN--Fe]
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6796
_journal_page_last               6803
_journal_paper_doi               10.1039/D3NJ00049D
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'2(C84 H78 Fe2 N6 P4 Ru), 7(F6 P), 2(C2 H3 N), H4 N'
_chemical_formula_sum            'C172 H166 F42 Fe4 N15 P15 Ru2'
_chemical_formula_weight         4131.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.15 svn.rb8c1d4dc for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.278(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.313(9)
_cell_length_b                   14.540(4)
_cell_length_c                   38.850(11)
_cell_measurement_reflns_used    23805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.1065
_cell_volume                     18181(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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            60420
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.107
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'RIGAKU/MSC(2004),CrystalClear Version 1.3.6'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             8392
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.830
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         15966
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1653P)^2^+98.2885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2731
_refine_ls_wR_factor_ref         0.2945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12822
_reflns_number_total             15966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00049d2.cif
_cod_data_source_block           ccdc2233238
_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 7062344--7062348.cif.
;
_cod_original_cell_volume        18182(8)
_cod_database_code               7062347
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1C} of N1, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H1B,H1D} of N1
2. Restrained distances
 C86-N7
 1.15 with sigma of 0.01
 C85-C86
 1.45 with sigma of 0.01
 C85-N7
 2.45 with sigma of 0.02
 P5-F1 = P5-F2 = P5-F3 = P5-F4 = P5-F6 = P5-F5
 1.58 with sigma of 0.01
 F1-F5 = F3-F6 = F2-F4
 3.16 with sigma of 0.02
 F1-F2 = F1-F3 = F1-F4 = F1-F6 = F2-F3 = F2-F5 = F2-F6 = F3-F5 = F3-F4
 2.23 with sigma of 0.02
 P5-F2A = P5-F3A = P5-F4A = P5-F6A
 1.58 with sigma of 0.01
 F3A-F6A = F2A-F4A
 3.16 with sigma of 0.02
 F1-F6A = F1-F4A = F1-F3A = F1-F2A = F6A-F4A = F6A-F2A = F6A-F5 = F4A-F5 = F4A-
 F3A
 2.23 with sigma of 0.02
 P7-F13 = P7-F14 = P7-F15 = P7-F16 = P7-F17 = P7-F18
 1.58 with sigma of 0.01
 F13-F18 = F15-F16 = F14-F17
 3.16 with sigma of 0.02
 F13-F16 = F13-F14 = F13-F15 = F13-F17 = F16-F14 = F16-F18
 2.23 with sigma of 0.02
 F16-F17 = F14-F18 = F14-F15
 2.23 with sigma of 0.02
 P7A-F13A = P7A-F14A = P7A-F15A = P7A-F16A = P7A-F17A = P7A-F18A
 1.58 with sigma of 0.01
 F16A-F18A = F17A-F14A = F15A-F13A
 3.16 with sigma of 0.02
 F13A-F18A = F13A-F14A = F13A-F16A = F13A-F17A = F18A-F14A = F18A-F15A
 2.23 with sigma of 0.02
 F18A-F17A = F14A-F15A = F14A-F16A
 2.23 with sigma of 0.02
 P8-F19 = P8-F20 = P8-F21
 1.58 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P5 \\sim P6 \\sim P8 \\sim F1 \\sim F5 \\sim F2 \\sim F3 \\sim F4 \\sim F6
\\sim F2A \\sim F3A \\sim F4A \\sim F6A \\sim F7 \\sim F8 \\sim F9 \\sim F10
\\sim F11 \\sim F12 \\sim F19 \\sim F20 \\sim F21 \\sim P7 \\sim F13 \\sim F14
\\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim P7A \\sim F13A \\sim F14A \\sim
F15A \\sim F16A \\sim F17A \\sim F18A: within 1.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.8A
C85 \\sim C86 \\sim N7: within 1.8A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.8A
Uanis(C39) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F9) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F17) \\sim Ueq, Uanis(F17A) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(F15A)
\\sim Ueq, Uanis(F18A) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 P7, F13, F14, F15, F16, F17, F18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: F2(0.5) F3(0.5) F4(0.5) F6(0.5) F2A(0.5) F3A(0.5) F4A(0.5)
 F6A(0.5) P7(0.6) F13(0.6) F14(0.6) F15(0.6) F16(0.6) F17(0.6) F18(0.6)
 P7A(0.4) F13A(0.4) F14A(0.4) F15A(0.4) F16A(0.4) F17A(0.4) F18A(0.4) N1(0.5)
 H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Riding coordinates:
 C50(H50), C51(H51), C63(H63), C64(H64), C65(H65), C66(H66), N1(H1A,H1B,H1C,H1D)
6.b Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58)
6.c Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C59(H59A,H59B), C60(H60A,H60B)
6.d Me refined with riding coordinates:
 C85(H85A,H85B,H85C)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
  C20(H20), C21(H21), C22(H22), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C52(H52), C53(H53), C62(H62),
 C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
  C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
;
_shelx_res_checksum              13258
_olex2_submission_special_instructions 'No special instructions were received'