Crystal structure of trans-tetrakis(acetonitrile-κN)bis(triphenylphosphine-κP)ruthenium(II) dihexafluorophosphate - dichloroform (1/2), C46H44Cl6F12N4P4Ru
Junwei, Zheng; Lu, Xiu Lian; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 425–427; doi:10.1515/ncrs-2018-0430

data_8105668
_publ_section_title
;
 Crystal structure of
 trans-tetrakis(acetonitrile-\kN)bis(triphenylphosphine-\kP)ruthenium(II)
 dihexafluorophosphate - dichloroform (1/2), C46H44Cl6F12N4P4Ru
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              425
_journal_page_last               427
_journal_paper_doi               10.1515/ncrs-2018-0430
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C44 H42 N4 P2 Ru, 2(F6 P), 2(C H Cl3)'
_chemical_formula_sum            'C46 H44 Cl6 F12 N4 P4 Ru'
_chemical_formula_weight         1318.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.319(2)
_cell_length_b                   16.7358(5)
_cell_length_c                   22.6972(16)
_cell_measurement_reflns_used    1376
_cell_measurement_temperature    235
_cell_measurement_theta_max      62.364
_cell_measurement_theta_min      20.726
_cell_volume                     5439.2(9)
_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      235.38
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22410
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.708
_diffrn_reflns_theta_min         3.895
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.861
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1343 before and 0.0645 after correction. The 
Ratio of minimum to maximum transmission is 0.8748. The \l/2 
correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     422
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0411P)^2^+41.4756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2515
_reflns_number_total             4348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0430_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        5439.1(9)
_cod_database_code               8105668
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.356
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F9) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: F9(0.5) F7(0.5) F4(0.5) F1(0.5) F2(0.5) F5(0.5) F6(0.5) F8(0.5)
5.a Ternary CH refined with riding coordinates:
 C23(H23)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C5(H5), C4(H4), C1(H1), C14(H14), C9(H9),
 C17(H17), C11(H11), C18(H18), C15(H15), C3(H3), C10(H10), C2(H2)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
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