Group VIII coordination complexes of bidentate P^N ligands bearing π-extended quinoline or phenanthridine N-heterocycles
Mondal, Rajarshi; Braun, Jason D.; Lozada, Issiah B.; Nickel, Rachel; van Lierop, Johan; Herbert, David E.; New Journal of Chemistry 45 (2021) 4427–4436; doi:10.1039/D1NJ00254F

data_7060387
_publ_section_title
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 Group VIII coordination complexes of bidentate P^N ligands bearing
 \p-extended quinoline or phenanthridine N-heterocycles
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_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4427
_journal_page_last               4436
_journal_paper_doi               10.1039/D1NJ00254F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C78 H60 N3 P3 Ru, 2(F6 P)'
_chemical_formula_sum            'C78 H60 F12 N3 P5 Ru'
_chemical_formula_weight         1523.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-08
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                71.268(2)
_cell_angle_beta                 78.496(2)
_cell_angle_gamma                76.944(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8277(6)
_cell_length_b                   14.1535(7)
_cell_length_c                   21.4310(10)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.47
_cell_volume                     3832.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.632
_diffrn_reflns_theta_min         2.310
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0747 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.9437.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         3.839
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         17778
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+14.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13034
_reflns_number_total             17778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00254f2.cif
_cod_data_source_block           deh241
_cod_depositor_comments
'Adding full bibliography for 7060382--7060389.cif.'
_cod_database_code               7060387
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.872
_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. Restrained distances
 P5A-F7A = P5A-F8A = P5A-F9A = P5A-F10A = P5A-F11A = P5A-F12A
 1.54645 with sigma of 0.04
 F7A-F10A = F8A-F11A = F9A-F12A
 3.0929 with sigma of 0.04
 P5A-F7A \\sim P5A-F8A \\sim P5A-F9A \\sim P5A-F10A \\sim P5A-F11A \\sim
P5A-F12A
 with sigma of 0.02
 F9A-F12A \\sim F8A-F11A \\sim F7A-F10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F7A) = Uanis(F8A) = Uanis(F9A) = Uanis(F10A) = Uanis(F11A) = Uanis(F12A)
Uanis(F7B) = Uanis(F8B) = Uanis(F9B) = Uanis(F10B) = Uanis(F11B) = Uanis(F12B)
4. Others
 Sof(P5B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(1)
 Sof(P5A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(1)
 1(DANG)=FVAR(2)
 1(DANG)=2*FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C37(H37),
 C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
 C58(H58), C63(H63), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
  C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C66(H66A,H66B,H66C)
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_shelx_res_checksum              71918
_shelx_hkl_checksum              45257
_shelx_fab_checksum              25508
_olex2_submission_special_instructions 'No special instructions were received'