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_7043427
_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         'C29 H27 N5 O Ru, 2(F6 P), 2(H2 O)'
_chemical_formula_sum            'C29 H31 F12 N5 O3 P2 Ru'
_chemical_formula_weight         888.60
_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   mixed
_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                82.409(11)
_cell_angle_beta                 65.522(13)
_cell_angle_gamma                64.36(2)
_cell_formula_units_Z            2
_cell_length_a                   11.563(4)
_cell_length_b                   12.841(5)
_cell_length_c                   13.303(5)
_cell_measurement_reflns_used    4837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      2.37
_cell_volume                     1618.0(11)
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32212
_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         27.513
_diffrn_reflns_theta_min         1.685
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_correction_T_min  0.7149
_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    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4962
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01847a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        1618.1(10)
_cod_database_code               7043427
_shelx_shelxl_version_number     2016/6
_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, All O(H,H) groups
2. Restrained distances
 P2A-F7A = P2A-F11A = P2A-F12A = P2A-F9A = P2A-F10A = P2A-F8A
 1.59684 with sigma of 0.01
 F7A-F8A = F7A-F9A = F7A-F10A = F7A-F12A = F12A-F8A = F12A-F10A = F12A-F11A =
 F10A-F9A = F10A-F11A = F8A-F9A
 2.257932 with sigma of 0.015
 P2-F7 = P2-F11 = P2-F12 = P2-F9 = P2-F10 = P2-F8
 1.59684 with sigma of 0.01
 F7-F8 = F7-F9 = F7-F10 = F7-F12 = F12-F8 = F12-F10 = F12-F11 = F10-F9 = F10-
 F11 = F8-F9
 2.257932 with sigma of 0.015
3. Rigid bond restraints
 P2A, F7A, F11A, F12A, F9A, F10A, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, F7, F11, F12, F9, F10, F8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F7 \\sim F11: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
F10 \\sim F8: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
F7A \\sim F11A: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
F12A \\sim F9A: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
F8A \\sim F10A: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
F9 \\sim F12: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim
Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.414*FVAR(2)
 Sof(P2A)=Sof(F8A)=Sof(F7A)=Sof(F12A)=Sof(F10A)=Sof(F11A)=Sof(F9A)=1-FVAR(2)
 Sof(P2)=Sof(F7)=Sof(F11)=Sof(F10)=Sof(F8)=Sof(F9)=Sof(F12)=FVAR(2)
6.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B)
6.b Rotating group:
 O1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C17(H17), C14(H14), C9(H9), C24(H24), C28(H28), C12(H12), C16(H16),
 C27(H27), C26(H26), C2(H2), C22(H22), C3(H3), C21(H21), C23(H23), C15(H15),
 C4(H4), C10(H10), C11(H11)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              7505
_olex2_submission_special_instructions 'No special instructions were received'