Synthesis, characterization and biological evaluation of cationic organoruthenium(ii) fluorene complexes: influence of the nature of the counteranion.
Haghdoost, Mohammad Mehdi; Golbaghi, Golara; Guard, Juliette; Sielanczyk, Sarah; Patten, Shunmoogum A.; Castonguay, Annie; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13396–13405; doi:10.1039/c9dt00143c

data_7700889
_publ_section_title
;
 Synthesis, characterization and biological evaluation of cationic
 organoruthenium(ii) fluorene complexes: influence of the nature of the
 counteranion.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13396
_journal_page_last               13405
_journal_paper_doi               10.1039/c9dt00143c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 B, C25 H20 Cl N2 Ru'
_chemical_formula_sum            'C49 H40 B Cl N2 Ru'
_chemical_formula_weight         804.16
_chemical_name_common            3[BPh4]
_chemical_name_systematic        3[BPh4]
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-06 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2318(7)
_cell_length_b                   13.1222(5)
_cell_length_c                   33.2897(14)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    150
_cell_measurement_theta_max      56.875
_cell_measurement_theta_min      3.657
_cell_volume                     7685.9(5)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            51225
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.431
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_T_max  0.3708
_exptl_absorpt_correction_T_min  0.1730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1466 before and 0.0883 after correction. The Ratio of minimum to maximum transmission is 0.4666. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       Block
_exptl_crystal_F_000             3312
_exptl_crystal_recrystallization_method 'crystallized from DCM/Methanol'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00038(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0751
_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^)+(0.0362P)^2^+65.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6581
_reflns_number_total             7900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00143c2.cif
_cod_data_source_block           3[BPh4]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700887--7700889.cif.
;
_cod_database_code               7700889
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.709
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C7B \\sim C8B
\\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B
\\sim C16B \\sim C17B \\sim C18B \\sim C19B: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.02
3. Same fragment restrains
{C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A}
sigma for 1-2: 0.02, 1-3: 0.04
as
{C7B, C8B, C9B, C10B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B}
4. Others
 Sof(C7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(C10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=
 Sof(H12B)=Sof(C13B)=Sof(C14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=
 Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C19A(H19A,H19B), C19B(H19C,H19D)
5.b Aromatic/amide H refined with riding coordinates:
 C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C), C8C(H8C), C9C(H9C),
 C10C(H10C), C11C(H11C), C12C(H12C), C14C(H14C), C15C(H15C), C16C(H16C),
 C17C(H17C), C18C(H18C), C20C(H20C), C21C(H21C), C22C(H22C), C23C(H23C),
 C24C(H24C), C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C8A(H8A), C11A(H11A), C12A(H12A),
 C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C8B(H8B), C11B(H11B),
 C12B(H12B), C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B)
5.c Fitted hexagon refined as free rotating group:
 C7A(C8A,C9A,C10A,C11A,C12A)
;
_shelx_res_checksum              8335
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'