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_7061255
_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, 3(F6 P), C3 H6 O'
_chemical_formula_sum            'C103 H116 F18 Fe2 N6 O P7 Ru'
_chemical_formula_weight         2225.57
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc24rr2r
_audit_creation_date             2022-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-26 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.184(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0216(17)
_cell_length_b                   32.214(5)
_cell_length_c                   27.028(4)
_cell_measurement_reflns_used    30102
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.0427
_cell_volume                     11222(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            78718
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.240
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5913
_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    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             4588
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         19681
_refine_ls_number_restraints     982
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+14.7695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16958
_reflns_number_total             19681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05900a2.cif
_cod_data_source_block           b
_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               7061255
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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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
 P5-F1 = P5-F2 = P5-F3 = P5-F4 = P5-F5 = P5-F6
 1.58 with sigma of 0.01
 F2-F3 = F4-F1 = F5-F6
 3.16 with sigma of 0.02
 F1-F3 = F1-F6 = F1-F5 = F1-F2 = F6-F2 = F6-F4 = F6-F3
 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 = F16-F17 = F15-F14
 3.16 with sigma of 0.02
 F15-F13 = F15-F17 = F15-F18 = F15-F16 = F17-F13 = F17-F14 = F17-F18
 2.23 with sigma of 0.02
 P6-F7 = P6-F8 = P6-F9 = P6-F10 = P6-F11 = P6-F12
 1.58 with sigma of 0.01
 F9-F10 = F7-F8 = F11-F12
 3.16 with sigma of 0.02
 F8-F9 = F8-F12 = F8-F10 = F8-F11 = F9-F12 = F9-F7 = F9-F11
 2.23 with sigma of 0.02
 P6A-F7A = P6A-F8A = P6A-F9A = P6A-F10A = P6A-F11A = P6A-F12A
 1.58 with sigma of 0.01
 F9A-F10A = F7A-F8A = F11A-F12A
 3.16 with sigma of 0.02
 F8A-F9A = F8A-F12A = F8A-F10A = F8A-F11A = F9A-F12A = F9A-F7A = F9A-F11A
 2.23 with sigma of 0.02
 F14A-F15A = F13A-F18A = F16A-F17A
 3.16 with sigma of 0.02
 F13A-F17A = F13A-F15A = F13A-F16A = F13A-F14A = F17A-F15A = F17A-F18A
 2.23 with sigma of 0.02
 F17A-F16A = F15A-F18A = F15A-F16A
 2.23 with sigma of 0.02
 C39-C40 \\sim C39-C40A
 with sigma of 0.02
 C39-C42 \\sim C39-C42A
 with sigma of 0.02
 C39-C41 \\sim C39-C41A
 with sigma of 0.02
 P7-F17 \\sim P7A-F17A
 with sigma of 0.02
 P7-F18 \\sim P7A-F18A
 with sigma of 0.02
 F17-F18 \\sim F17A-F18A
 with sigma of 0.04
 F15-F17 \\sim F15A-F17A
 with sigma of 0.04
 P7-F14 \\sim P7A-F14A
 with sigma of 0.02
 F16-F18 \\sim F16A-F18A
 with sigma of 0.04
 F14-F15 \\sim F14A-F15A
 with sigma of 0.04
 F14-F17 \\sim F14A-F17A
 with sigma of 0.04
 P7-F15 \\sim P7A-F15A
 with sigma of 0.02
 P7-F16 \\sim P7A-F16A
 with sigma of 0.02
 P7-F13 \\sim P7A-F13A
 with sigma of 0.02
 F14-F16 \\sim F14A-F16A
 with sigma of 0.04
 F14-F18 \\sim F14A-F18A
 with sigma of 0.04
 F15-F16 \\sim F15A-F16A
 with sigma of 0.04
 F15-F18 \\sim F15A-F18A
 with sigma of 0.04
 F16-F17 \\sim F16A-F17A
 with sigma of 0.04
 F13-F14 \\sim F13A-F14A
 with sigma of 0.04
 F13-F15 \\sim F13A-F15A
 with sigma of 0.04
 F13-F16 \\sim F13A-F16A
 with sigma of 0.04
 F13-F17 \\sim F13A-F17A
 with sigma of 0.04
 F13-F18 \\sim F13A-F18A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P7A \\sim F13A \\sim F14A \\sim F15A \\sim F16A \\sim F17A \\sim F18A \\sim
C41A \\sim C40A \\sim C42A \\sim P7 \\sim F13 \\sim F14 \\sim F15 \\sim F16
\\sim F17 \\sim F18: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F7A) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(P7A)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F16) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F13A) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15A) \\sim Ueq,
Uanis(F16A) \\sim Ueq, Uanis(F17A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F18) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F9A) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(P7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O3) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C104)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F16, P7, F14, F13, F18, F17, F15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F13A, P7A, F14A, F18A, F17A, F15A, F16A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C102, O104, C101, C103
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C106, O3, C105, C104
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F9A, P6A, F7A, F8A, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F8, P6, F7, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1A, P5A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F6, P5, F1, F2, F3, F4, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(P7)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(2)
 Sof(P7A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(2)
 Fixed Sof: P5(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) P5A(0.5)
 F1A(0.5) F2A(0.5) F3A(0.5) F4A(0.5) F5A(0.5) F6A(0.5) P6(0.5) F7(0.5) F8(0.5)
 F9(0.5) F10(0.5) F11(0.5) F12(0.5) P6A(0.5) F7A(0.5) F8A(0.5) F9A(0.5)
 F10A(0.5) F11A(0.5) F12A(0.5) O104(0.5) C101(0.5) H10A(0.5) H10B(0.5)
 H10C(0.5) C102(0.5) C103(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C106(0.5) O3(0.5)
 C105(0.5) H10G(0.5) H10H(0.5) H10I(0.5) C104(0.5) H10J(0.5) H10K(0.5) H10L(0.5)
6.a Riding coordinates:
 C101(H10A,H10B,H10C), C103(H10D,H10E,H10F)
6.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)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C75(H75A,H75B), C76(H76A,H76B)
6.d Me refined with riding coordinates:
 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), C104(H10J,H10K,H10L)
6.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)
6.f Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C41A(H41D,H41E,
 H41F), C40A(H40D,H40E,H40F), C42A(H42D,H42E,H42F), C105(H10G,H10H,H10I)
;
_shelx_res_checksum              90032
_shelx_fab_checksum              93343
_olex2_submission_special_instructions 'No special instructions were received'