1,3-Dimethyl-4-(diphenylphosphino)imidazolium Triflate: A Functionalized Ionic Liquid with Ambivalent Coordination Capability
Ruiz, Javier; Mesa, Alejandro F.; Sol, Daniel; Organometallics 34 (2015) 5129–; doi:10.1021/acs.organomet.5b00722

data_4087917
_publ_section_title
;
 1,3-Dimethyl-4-(diphenylphosphino)imidazolium Triflate: A Functionalized
 Ionic Liquid with Ambivalent Coordination Capability
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5129
_journal_paper_doi               10.1021/acs.organomet.5b00722
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H36 Cl N4 O P2 Rh, 2(C F3 O3 S)'
_chemical_formula_sum            'C37 H36 Cl F6 N4 O7 P2 Rh S2'
_chemical_formula_weight         1027.12
_chemical_name_systematic        DS-96
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-02T17:35:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.0744(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3407(2)
_cell_length_b                   19.9152(5)
_cell_length_c                   25.3728(5)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.2
_cell_measurement_wavelength     0.71073
_cell_volume                     4172.81(17)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.010441
_diffrn_orient_matrix_UB_12      -0.048356
_diffrn_orient_matrix_UB_13      0.010542
_diffrn_orient_matrix_UB_21      0.120578
_diffrn_orient_matrix_UB_22      0.00376
_diffrn_orient_matrix_UB_23      0.003448
_diffrn_orient_matrix_UB_31      0.003958
_diffrn_orient_matrix_UB_32      0.012996
_diffrn_orient_matrix_UB_33      0.03823
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            94360
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.603
_diffrn_reflns_theta_min         1.621
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.73
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 5008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     618
_refine_ls_number_reflns         12754
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.99
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.99
_reflns_number_gt                11239
_reflns_number_total             12754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00722_si_002.cif
_cod_data_source_block           '[10](OTf)2'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4087917
_shelx_estimated_absorpt_t_min   0.88
_shelx_estimated_absorpt_t_max   0.958