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_7060388
_publ_section_title
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 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         'C78 H60 Fe N3 P3, 2(F6 P)'
_chemical_formula_sum            'C78 H60 F12 Fe N3 P5'
_chemical_formula_weight         1477.99
_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             2020-06-03
_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                72.199(5)
_cell_angle_beta                 78.434(5)
_cell_angle_gamma                75.908(5)
_cell_formula_units_Z            2
_cell_length_a                   13.9092(14)
_cell_length_b                   14.2075(14)
_cell_length_c                   21.287(2)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.46
_cell_volume                     3848.3(7)
_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 0.996
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            134036
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.819
_diffrn_reflns_theta_max         24.819
_diffrn_reflns_theta_min         2.314
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0577 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.9346.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.424
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         13221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.1005
_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^)+(0.0200P)^2^+40.2656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11120
_reflns_number_total             13221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00254f2.cif
_cod_data_source_block           deh133
_cod_depositor_comments
'Adding full bibliography for 7060382--7060389.cif.'
_cod_database_code               7060388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.890
_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. 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)
3. 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)
4.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)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              70907
_shelx_hkl_checksum              43120
_shelx_fab_checksum              11293
_olex2_submission_special_instructions 'No special instructions were received'