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_7231193
_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         'C38 H29 Cl2 N3 P2 Pt, C H Cl3'
_chemical_formula_sum            'C39 H30 Cl5 N3 P2 Pt'
_chemical_formula_weight         974.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-03-24 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2544(3)
_cell_length_b                   12.3816(4)
_cell_length_c                   28.9853(11)
_cell_measurement_reflns_used    12932
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.6430
_cell_measurement_theta_min      2.1120
_cell_volume                     3680.1(2)
_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 (Sheldrick, 2015)'
_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    -49.00  70.00   0.50   16.00    --  -20.00  72.00-180.00  238
  2  \w    -38.50  40.00   0.50   16.00    --  -20.00  72.00-108.00  157
  3  \w    -30.00   0.00   0.50   16.00    --  -20.00 -72.00-108.00   60
  4  \w    -58.50  39.00   0.50   16.00    --  -20.00   0.00 -36.00  195
  5  \w    -74.50 -44.00   0.50   16.00    --  -20.00 -72.00 -36.00   61
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0289072000
_diffrn_orient_matrix_UB_12      0.0486333000
_diffrn_orient_matrix_UB_13      0.0078754000
_diffrn_orient_matrix_UB_21      0.0581406000
_diffrn_orient_matrix_UB_22      0.0284139000
_diffrn_orient_matrix_UB_23      -0.0053407000
_diffrn_orient_matrix_UB_31      -0.0238104000
_diffrn_orient_matrix_UB_32      0.0102409000
_diffrn_orient_matrix_UB_33      -0.0225689000
_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  0.0751
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.645
_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    4.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85198
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.072
_refine_diff_density_max         3.048
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6484
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0375P)^2^+58.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6092
_reflns_number_total             6484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra04086a2.cif
_cod_data_source_block           msb-rk-156_mo
_cod_database_code               7231193
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C39H29N3P2PtCl2
_reflns_odcompleteness_completeness 94.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.08
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.676(16)
 0.324(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C30(H30), C29(H29), C28(H28), C26(H26), C25(H25),
 C24(H24), C23(H23), C22(H22), C6(H6), C4(H4), C3(H3), C5(H5), C38(H38),
 C37(H37), C36(H36), C35(H35), C34(H34), C10(H10), C11(H11), C12(H12), C13(H13),
  C14(H14), C20(H20), C19(H19), C18(H18), C17(H17), C16(H16)
4.c Fitted hexagon refined as free rotating group:
 C27(C32,C31,C30,C29,C28), C21(C26,C25,C24,C23,C22), C33(C38,C37,C36,C35,C34),
 C9(C10,C11,C12,C13,C14), C15(C20,C19,C18,C17,C16)
;
_shelx_res_checksum              897
_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 3.849
_oxdiff_exptl_absorpt_empirical_full_min 0.573