Influence of electronic spin and spin-orbit coupling on decoherence in mononuclear transition metal complexes.
Graham, Michael J.; Zadrozny, Joseph M.; Shiddiq, Muhandis; Anderson, John S.; Fataftah, Majed S.; Hill, Stephen; Freedman, Danna E.; Journal of the American Chemical Society 136 (2014) 7623–7626; doi:10.1021/ja5037397

data_4121834
_publ_section_title
;
 Influence of electronic spin and spin-orbit coupling on decoherence in
 mononuclear transition metal complexes.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7623
_journal_page_last               7626
_journal_paper_doi               10.1021/ja5037397
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C6 N6 Ru, 3(C24 H20 P), 2(C H2 Cl2), 3(C H Cl3), H1.68 C Cl2.32'
_chemical_formula_sum            'C84 H68.68 Cl15.32 N6 P3 Ru'
_chemical_formula_weight         1899.29
_chemical_name_systematic
'tris(tetraphenylphosphonium) hexacyanoruthenate(III)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.4650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7221(9)
_cell_length_b                   15.0978(6)
_cell_length_c                   25.3767(13)
_cell_measurement_temperature    100(2)
_cell_volume                     8621.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.09
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            70928
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.147
_diffrn_reflns_theta_min         1.763
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0857 after correction.
The Ratio of minimum to maximum transmission is 0.8986.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             3850
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 7762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         18493
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0427P)^2^+15.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                17137
_reflns_number_total             18493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5037397_si_002.cif
_cod_data_source_block           jz17
_cod_depositor_comments
'Adding full bibliography for 4121833--4121834.cif.'
_cod_database_code               4121834
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl6-Cl5 \\sim Cl5-Cl4 \\sim Cl4-Cl6
 with sigma of 0.01
 C200-Cl5 \\sim C200-Cl6 \\sim C200-Cl4
 with sigma of 0.01
 Cl18-Cl17 \\sim Cl16-Cl15 \\sim Cl7A-Cl4A \\sim Cl7B-Cl4A
 with sigma of 0.01
3. Others
 Sof(Cl4A)=1-FVAR(1)
 Sof(Cl7A)=Sof(Cl7B)=0.5*(1-FVAR(2))
 Sof(Cl6)=Sof(Cl5)=Sof(Cl4)=FVAR(1)
 Sof(Cl14)=1-FVAR(2)
 Sof(Cl13)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C31(H31), C44(H44), C59(H59), C60(H60), C61(H61), C64(H64),
 C71(H71), C72(H72), C75(H75), C76(H76), C80(H80), C84(H84), C94(H94),
 C102(H102), C104(H104), C109(H109), C115(H115), C135(H135), C28(H28), C29(H29),
  C36(H36), C39(H39), C41(H41), C43(H43), C47(H47), C51(H51), C53(H53),
 C54(H54), C58(H58), C65(H65), C69(H69), C70(H70), C73(H73), C74(H74), C78(H78),
  C81(H81), C82(H82), C83(H83), C85(H85), C87(H87), C90(H90), C93(H93),
 C96(H96), C97(H97), C99(H99), C100(H100), C101(H101), C103(H103), C105(H105),
 C107(H107), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C117(H117), C126(H126), C11(H11), C3(H3)
;
_shelx_res_checksum              93644
_shelx_hkl_checksum              3673
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'