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_7041552
_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         'C46 H39 N9 Ru2, 2(C H2 Cl2), B1 F4'
_chemical_formula_sum            'C48 H43 B Cl4 F4 N9 Ru2'
_chemical_formula_weight         1176.66
_chemical_properties_physical    ', Moisture-sensitive'
_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_update_record
;
2016-11-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                100.4935(15)
_cell_angle_beta                 93.5825(17)
_cell_angle_gamma                93.8681(16)
_cell_formula_units_Z            2
_cell_length_a                   10.0314(3)
_cell_length_b                   13.5259(4)
_cell_length_c                   18.1472(5)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.605
_cell_measurement_theta_min      2.263
_cell_volume                     2408.56(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      99.96
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70100
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.840
_diffrn_reflns_theta_min         1.144
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0980 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.8936.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1182
_exptl_crystal_recrystallization_method
'Solution of dichloromethane was layered with dry hexanes for slow diffusion.'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.982
_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         15053
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0705P)^2^+9.0054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10564
_reflns_number_total             15053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04328c2.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
'Adding full bibliography for 7041550--7041554.cif.'
_cod_database_code               7041552
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C47 \\sim Cl2A-C47 \\sim Cl2-C47
 with sigma of 0.02
 Cl3A-C48A \\sim Cl4A-C48A \\sim Cl4-C48 \\sim Cl3-C48
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C48 \\sim C48A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
B1 \\sim F4 \\sim F1 \\sim F3 \\sim F2 \\sim B1A \\sim F3A \\sim F4A \\sim F2A
\\sim F1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl4) = Uanis(Cl3) = Uanis(Cl4A) = Uanis(Cl3A) = Uanis(Cl1) = Uanis(Cl2) =
Uanis(Cl2A)
4. Others
 Sof(Cl3A)=Sof(Cl4A)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
 Sof(Cl2A)=Sof(H47C)=Sof(H47D)=1-FVAR(2)
 Sof(Cl2)=Sof(H47A)=Sof(H47B)=FVAR(2)
 Sof(B1A)=Sof(F3A)=Sof(F4A)=Sof(F2A)=Sof(F1A)=1-FVAR(3)
 Sof(B1)=Sof(F4)=Sof(F1)=Sof(F3)=Sof(F2)=FVAR(3)
5.a Free rotating group:
 B1(F4,F1,F3,F2), B1A(F3A,F4A,F2A,F1A)
5.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C47(H47C,H47D), C48(H48A,H48B), C48A(H48C,H48D)
5.c 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)
5.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              13428
_olex2_submission_special_instructions 'No special instructions were received'