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_7719456
_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         'C20 H27 N4 O3 P Ru, C32 H12 B F24, 2[C4H8O]'
_chemical_formula_sum            'C60 H55 B F24 N4 O5 P Ru'
_chemical_formula_weight         1510.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-06-06
_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                90
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.026(3)
_cell_length_b                   14.2764(18)
_cell_length_c                   34.330(13)
_cell_measurement_reflns_used    2388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.6900
_cell_measurement_theta_min      2.6920
_cell_volume                     6865(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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1819
_diffrn_reflns_av_unetI/netI     0.2101
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            31934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.828
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.768
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.335
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         12549
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.2413
_refine_ls_R_factor_gt           0.1278
_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^)+(0.1929P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3208
_refine_ls_wR_factor_ref         0.4115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4160
_reflns_number_total             12549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01437a2.cif
_cod_data_source_block           x1307
_cod_depositor_comments
'Adding full bibliography for 7719452--7719457.cif.'
_cod_database_code               7719456
_shelx_shelxl_version_number     2018/3
_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
 C28-F1 \\sim C28-F1A
 with sigma of 0.02
 C28-F2 \\sim C28-F2A
 with sigma of 0.02
 C28-F3 \\sim C28-F3A
 with sigma of 0.02
 F8-C35 \\sim F8A-C35
 with sigma of 0.02
 F7-C35 \\sim F7A-C35
 with sigma of 0.02
 F9-C35 \\sim F9A-C35
 with sigma of 0.02
 F6-C27 \\sim F6A-C27
 with sigma of 0.02
 F4-C27 \\sim F4A-C27
 with sigma of 0.02
 F5-C27 \\sim F5A-C27
 with sigma of 0.02
3. Rigid bond restraints
 F19, C43, F20, F21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 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(F3) = Uanis(F3A) = Uanis(F2) = Uanis(F2A) = Uanis(F1) = Uanis(F1A) =
Uanis(C28)
Uanis(F8A) = Uanis(F9) = Uanis(F9A) = Uanis(F7) = Uanis(F7A) = Uanis(F8)
Uanis(F8A) = Uanis(F9) = Uanis(F9A) = Uanis(F7) = Uanis(F7A) = Uanis(F8) =
Uanis(C35)
Uanis(F5A) = Uanis(F5) = Uanis(F6A) = Uanis(F6) = Uanis(F4A) = Uanis(F4) =
Uanis(C27)
5. Others
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(2)
 Sof(F8)=Sof(F7)=Sof(F9)=FVAR(2)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(3)
 Sof(F6)=Sof(F4)=Sof(F5)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C34(H34), C26(H26), C38(H38), C30(H30), C50(H50), C22(H22),
 C42(H42), C32(H32), C40(H40), C24(H24), C48(H48), C11(H11), C12(H12), C10(H10),
  C8(H8), C9(H9), C5(H5)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C6(H6A,H6B,
 H6C), C18(H18A,H18B,H18C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 298 electrons were 
found in a volume of 1306\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2[C4H8O] per Formula Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76102
_shelx_hkl_checksum              92271
_shelx_fab_checksum              49328
_olex2_submission_special_instructions 'No special instructions were received'