Synthesis, characterization and solution behavior of a systematic series of pentapyridyl-supported RuII complexes: Comparison to bimetallic analogs
Park, Sungho V.; Berry, John F.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01847A

data_7043426
_publ_section_title
;
 Synthesis, characterization and solution behavior of a systematic series
 of pentapyridyl-supported RuII complexes: Comparison to bimetallic
 analogs
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01847A
_journal_year                    2017
_chemical_formula_moiety         'C31 H28 N6 Ru, 2(F6 P)'
_chemical_formula_sum            'C31 H28 F12 N6 P2 Ru'
_chemical_formula_weight         875.60
_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     dual
_audit_creation_date             2017-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-16 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                110.34(2)
_cell_angle_beta                 108.484(13)
_cell_angle_gamma                90.749(14)
_cell_formula_units_Z            2
_cell_length_a                   11.443(4)
_cell_length_b                   12.524(4)
_cell_length_c                   13.131(5)
_cell_measurement_reflns_used    3317
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.85
_cell_measurement_theta_min      2.40
_cell_volume                     1657.3(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.444
_diffrn_reflns_theta_min         1.751
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.9517
_exptl_absorpt_correction_T_min  0.8505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5101
_reflns_number_total             6829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01847a2.cif
_cod_data_source_block           4
_cod_original_cell_volume        1657.3(11)
_cod_database_code               7043426
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C16(H16), C15(H15), C24(H24), C12(H12), C21(H21), C9(H9),
 C10(H10), C23(H23), C11(H11), C28(H28), C29(H29), C2(H2), C27(H27), C4(H4),
 C3(H3), C26(H26), C22(H22)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              41088
_olex2_submission_special_instructions 'No special instructions were received'