On the chemistry of <i>p</i>-cymene ruthenium iodide complexes: entry into octahedral phenylated ruthenium(II) complexes supported by chelating bidentate N,N'-donor ligands.
Quillian, Brandon; Marks, Allison; Musso, Kennedy; Durrell, George; Bazemore, Joseph; Padgett, Clifford W.; Fields, Alexis; Zurwell, Dane; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15025–15042; doi:10.1039/d5dt01437a

data_7719457
_publ_section_title
;
 On the chemistry of <i>p</i>-cymene ruthenium iodide complexes: entry
 into octahedral phenylated ruthenium(II) complexes supported by chelating
 bidentate N,N'-donor ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15025
_journal_page_last               15042
_journal_paper_doi               10.1039/d5dt01437a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C42 H58 N4 O3 P Ru, C32 H12 B F24'
_chemical_formula_sum            'C74 H70 B F24 N4 O3 P Ru'
_chemical_formula_weight         1662.19
_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
_audit_creation_date             2025-06-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-10 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                91.479(3)
_cell_angle_beta                 91.721(3)
_cell_angle_gamma                99.826(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5761(4)
_cell_length_b                   19.1778(7)
_cell_length_c                   21.8410(8)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    173
_cell_measurement_theta_max      21.0940
_cell_measurement_theta_min      2.1270
_cell_volume                     3948.5(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'clear dark Green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.171
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         13958
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0935
_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^)+(0.1782P)^2^+6.1704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.2957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9397
_reflns_number_total             13958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01437a2.cif
_cod_data_source_block           exp_131
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Green' was changed
to 'green' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719452--7719457.cif.
;
_cod_database_code               7719457
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.863
_diffrn_oxdiff_ac3_digest_hkl    01cc6b2dd2162f1bcdb4489dedc4495ffbc61a
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2-F3 \\sim F2A-F1A
 with sigma of 0.02
 F2-F1 \\sim F2A-F3A
 with sigma of 0.02
 C49-F2 \\sim C49-F2A
 with sigma of 0.04
 C49-F3 \\sim C49-F1A
 with sigma of 0.04
 C49-F1 \\sim C49-F3A
 with sigma of 0.04
 F3-F1 \\sim F1A-F3A
 with sigma of 0.04
 F20A-F19A \\sim F21-F20
 with sigma of 0.02
 F21A-F19A \\sim F19-F20
 with sigma of 0.02
 C73-F20A \\sim C73-F21
 with sigma of 0.04
 C73-F21A \\sim C73-F19
 with sigma of 0.04
 C73-F19A \\sim C73-F20
 with sigma of 0.04
 F20A-F21A \\sim F21-F19
 with sigma of 0.04
 C58-F10 \\sim C58-F11A
 with sigma of 0.02
 F11-F12 \\sim F12A-F10A
 with sigma of 0.02
 C58-F11 \\sim C58-F12A
 with sigma of 0.04
 C58-F12 \\sim C58-F10A
 with sigma of 0.04
 F7-C57 \\sim F8A-C57
 with sigma of 0.02
 F9-C57 \\sim F9A-C57
 with sigma of 0.02
 F8-C57 \\sim F7A-C57
 with sigma of 0.02
 F14A-C65 \\sim F15-C65
 with sigma of 0.02
 F15A-C65 \\sim F14-C65
 with sigma of 0.02
 C65-F13 \\sim C65-F13A
 with sigma of 0.02
 C74-F24 \\sim C74-F23A
 with sigma of 0.02
 C74-F22 \\sim C74-F22A
 with sigma of 0.02
 C74-F23 \\sim C74-F24A
 with sigma of 0.02
3. Rigid bond restraints
 C49, F1, F2, F3, F1A, F2A, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C73, F19A, F20A, F21A, F19, F20, F21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57, F7, F8, F9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C74, F22, F23, F24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, F10, F11, F12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F4, F5, F6, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, F10, F11, F12, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57, F7, F8, F9, F7A, F8A, F9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C65, F14A, F15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C65, F14A, F15A, F13, F14, F15, F13A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C74, F22, F23, F24, F22A, F23A, F24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C67, C68, C69, C70, C71, C72, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F9A) = Uanis(F7A) = Uanis(F8) = Uanis(F7) = Uanis(F8A) = Uanis(F9) =
Uanis(C57)
Uanis(F23A) = Uanis(F24) = Uanis(F24A) = Uanis(F23) = Uanis(F22A) = Uanis(F22)
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=1-FVAR(2)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
 Sof(F14)=Sof(F15)=Sof(F13A)=1-FVAR(5)
 Sof(F14A)=Sof(F15A)=Sof(F13)=FVAR(5)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(6)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C44(H44), C46(H46), C48(H48),
  C52(H52), C54(H54), C56(H56), C60(H60), C62(H62), C64(H64), C68(H68),
 C70(H70), C72(H72)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              98635
_shelx_hkl_checksum              84492
_olex2_submission_special_instructions 'No special instructions were received'