1,2,3-Triazole based bisphosphine, 5-(diphenylphosphanyl)-1-(2-(diphenylphosphanyl)-phenyl)-4-phenyl-1H-1,2,3-triazole: an ambidentate ligand with switchable coordination modes
Radhakrishna, Latchupatula; Pandey, Madhusudan K.; Balakrishna, Maravanji S.; RSC Advances 8 (2018) 25704–; doi:10.1039/C8RA04086A

data_7231195
_publ_section_title
;
 1,2,3-Triazole based bisphosphine,
 5-(diphenylphosphanyl)-1-(2-(diphenylphosphanyl)-phenyl)-4-phenyl-1H-1,2,3-triazole:
 an ambidentate ligand with switchable coordination modes
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              25704
_journal_paper_doi               10.1039/C8RA04086A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C48 H43 Cl N3 P2 Ru, Cl'
_chemical_formula_sum            'C48 H43 Cl2 N3 P2 Ru'
_chemical_formula_weight         895.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-03-24 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                114.525(6)
_cell_angle_beta                 103.851(5)
_cell_angle_gamma                102.567(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7908(7)
_cell_length_b                   15.2107(10)
_cell_length_c                   15.2959(10)
_cell_measurement_reflns_used    10686
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.0430
_cell_measurement_theta_min      2.3240
_cell_volume                     2453.7(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  19.00   0.50   16.00    --  -20.00 -72.00 -36.00  258
  2  \w    -98.00  19.00   0.50   16.00    --  -20.00 -72.00-180.00  234
  3  \w   -105.50   1.00   0.50   16.00    --  -20.00   0.00-180.00  213
  4  \w    -35.00   3.00   0.50   16.00    --  -20.00 -72.00  36.00   76
  5  \w    -59.00 -28.50   0.50   16.00    --  -20.00  72.00-180.00   61
  6  \w    -39.00  -9.00   0.50   16.00    --  -20.00 -72.00-108.00   60
  7  \w   -110.00  25.00   0.50   16.00    --  -20.00   0.00 -36.00  270
  8  \w    -87.00  19.00   0.50   16.00    --  -20.00 -72.00 108.00  212
  9  \w    -59.00  35.50   0.50   16.00    --  -20.00  72.00 -36.00  189
 10  \w    -58.50  -3.00   0.50   16.00    --  -20.00  72.00  36.00  111
 11  \w    -44.00 -10.00   0.50   16.00    --  -20.00  72.00-108.00   68
 12  \w    -59.00 -28.50   0.50   16.00    --  -20.00  72.00 108.00   61
 13  \w    -94.00  30.50   0.50   16.00    --  -20.00   0.00  36.00  249
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0033733000
_diffrn_orient_matrix_UB_12      -0.0022783000
_diffrn_orient_matrix_UB_13      0.0446697000
_diffrn_orient_matrix_UB_21      -0.0219531000
_diffrn_orient_matrix_UB_22      -0.0548566000
_diffrn_orient_matrix_UB_23      -0.0289522000
_diffrn_orient_matrix_UB_31      0.0570210000
_diffrn_orient_matrix_UB_32      -0.0001024000
_diffrn_orient_matrix_UB_33      0.0133802000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1737
_diffrn_reflns_av_unetI/netI     0.1217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47691
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.587
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66130
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1238P)^2^+3.2828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5930
_reflns_number_total             8624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra04086a2.cif
_cod_data_source_block           msb-rk-205-Ru-Cym
_cod_original_cell_volume        2453.6(3)
_cod_database_code               7231195
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C48H33N3P2RuCl2
_cell_oxdiff_angle_alpha         114.525(6)
_cell_oxdiff_angle_beta          103.851(5)
_cell_oxdiff_angle_gamma         102.567(5)
_cell_oxdiff_length_a            12.7908(7)
_cell_oxdiff_length_b            15.2107(10)
_cell_oxdiff_length_c            15.2959(10)
_cell_oxdiff_measurement_reflns_used 10720
_cell_oxdiff_volume              2453.6(2)
_reflns_odcompleteness_completeness 92.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.02
_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.a Ternary CH refined with riding coordinates:
 C45(H45)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3), C28(H28), C38(H38), C43(H43), C13(H13), C14(H14),
 C22(H22), C5(H5), C24(H24), C40(H40), C26(H26), C19(H19), C23(H23), C10(H10),
 C44(H44), C30(H30), C20(H20), C18(H18), C29(H29), C31(H31), C41(H41), C16(H16),
  C34(H34), C25(H25), C32(H32), C12(H12), C37(H37), C36(H36), C35(H35),
 C11(H11), C17(H17)
2.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              89820
_shelx_fab_checksum              61338
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.909
_oxdiff_exptl_absorpt_empirical_full_min 0.512