Anilinopyridinate-supported Ru2(x+) (x = 5 or 6) paddlewheel complexes with labile axial ligands.
Corcos, Amanda R.; Berry, John F.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5532–5539; doi:10.1039/c6dt04328c

data_7041551
_publ_section_title
;
 Anilinopyridinate-supported Ru2(x+) (x = 5 or 6) paddlewheel complexes
 with labile axial ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5532
_journal_page_last               5539
_journal_paper_doi               10.1039/c6dt04328c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C94 H72 Ag2 F18 N16 O18 Ru4 S6, 4(C H2 Cl2)'
_chemical_formula_sum            'C98 H80 Ag2 Cl8 F18 N16 O18 Ru4 S6'
_chemical_formula_weight         3207.76
_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
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-11-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                110.553(3)
_cell_angle_beta                 103.963(3)
_cell_angle_gamma                96.890(3)
_cell_formula_units_Z            1
_cell_length_a                   12.9901(8)
_cell_length_b                   13.7169(9)
_cell_length_c                   18.0952(11)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.05
_cell_measurement_theta_min      2.74
_cell_volume                     2854.5(3)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1143
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            95216
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.176
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    10.517
_exptl_absorpt_correction_T_max  0.753555
_exptl_absorpt_correction_T_min  0.288853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1260 before and 0.0623 after correction.
 The Ratio of minimum to maximum transmission is 0.73.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 88696 reflections, Rint = 0.1143
 (51980 with I > 3sig(I), Rint = 0.1077)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.787
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         10542
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0822P)^2^+1.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9642
_reflns_number_total             10542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04328c2.cif
_cod_data_source_block           Compound6
_cod_depositor_comments
'Adding full bibliography for 7041550--7041554.cif.'
_cod_database_code               7041551
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1-C45A \\sim S1-C45
 with sigma of 0.02
 F3A-C45A \\sim F1A-C45A \\sim F1-C45 \\sim F2-C45 \\sim F2A-C45A \\sim F3-C45
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C45A) = Uanis(C45)
Uanis(F3A) = Uanis(F3)
Uanis(F1A) = Uanis(F1)
Uanis(F2A) = Uanis(F2)
Uanis(Ag1A) = Uanis(Ag1)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C45A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C45)=FVAR(1)
 Sof(Ag1A)=1-FVAR(2)
 Sof(Ag1)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44)
;
_shelx_res_checksum              8661
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'