Multistep Oxidation of Diethynyl Oligophenylamine-Bridged Diruthenium and Diiron Complexes.
Zhang, Jing; Guo, Shen-Zhen; Dong, Yu-Bao; Rao, Li; Yin, Jun; Yu, Guang-Ao; Hartl, František; Liu, Sheng Hua; Inorganic chemistry 56 (2017) 1001–1015; doi:10.1021/acs.inorgchem.6b02809

data_4344995
_publ_section_title
;
 Multistep Oxidation of Diethynyl Oligophenylamine-Bridged Diruthenium and
 Diiron Complexes.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1001
_journal_page_last               1015
_journal_paper_doi               10.1021/acs.inorgchem.6b02809
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C106 H100 N2 P4 Ru2, 3(C H2 Cl2)'
_chemical_formula_sum            'C109 H106 Cl6 N2 P4 Ru2'
_chemical_formula_weight         1982.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                77.951(5)
_cell_angle_beta                 89.872(5)
_cell_angle_gamma                80.650(5)
_cell_formula_units_Z            1
_cell_length_a                   9.848(3)
_cell_length_b                   14.954(5)
_cell_length_c                   16.443(6)
_cell_measurement_reflns_used    8968
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.061
_cell_measurement_theta_min      2.326
_cell_volume                     2335.4(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19652
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.128
_diffrn_reflns_theta_min         1.267
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0954 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.7229.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.850
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.1398
_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^)+(0.1500P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4097
_refine_ls_wR_factor_ref         0.4261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8480
_reflns_number_total             10847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02809_si_003.cif
_cod_data_source_block           140606a
_cod_depositor_comments          'Adding full bibliography for 4344995.cif.'
_cod_database_code               4344995
_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
 Cl1-C54 \\sim Cl1-C54B \\sim Cl2-C54B \\sim Cl2-C54 \\sim Cl4-C55 \\sim Cl3-C55
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C54B) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C54(0.55) H54A(0.55) H54B(0.55) C54B(0.45) H54C(0.45) H54D(0.45)
 C55(0.5) H55A(0.5) H55B(0.5) Cl3(0.5) Cl4(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C54(H54A,H54B), C54B(H54C,H54D), C55(H55A,H55B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C33(H33), C34(H34),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43)
5.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              98741
_shelx_hkl_checksum              20448
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'