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_7060385
_publ_section_title
;
 Group VIII coordination complexes of bidentate P^N ligands bearing
 \p-extended quinoline or phenanthridine N-heterocycles
;
_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         'C66 H54 N3 P3 Ru1, 1.5(F6 P1)'
_chemical_formula_sum            'C66 H54 F9 N3 P4.5 Ru'
_chemical_formula_weight         1300.55
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-08-06
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.9917(8)
_cell_length_b                   13.9917(8)
_cell_length_c                   18.8197(12)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.74
_cell_volume                     3190.7(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66182
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.605
_diffrn_reflns_theta_min         2.741
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1162 before and 0.0874 after correction.
The Ratio of minimum to maximum transmission is 0.7806.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       plate
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.614
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0817
_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^)+(0.0645P)^2^+22.1469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4153
_reflns_number_total             4905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00254f2.cif
_cod_data_source_block           deh322
_cod_depositor_comments
'Adding full bibliography for 7060382--7060389.cif.'
_cod_original_cell_volume        3190.7(4)
_cod_original_formula_sum        'C66 H54 F9 N3 P4.50 Ru'
_cod_database_code               7060385
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.769
_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 angles
 F3_$1-P3-F3_$2
 fixed at 90 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C16(H16), C12(H12), C22(H22), C13(H13), C19(H19), C18(H18), C20(H20),
 C14(H14), C21(H21), C1(H1), C3(H3), C15(H15), C9(H9), C2(H2)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46026
_shelx_hkl_checksum              77449
_shelx_fab_checksum              61868
_olex2_submission_special_instructions 'No special instructions were received'