New 1,2,3-triazole based bis- and trisphosphine ligands: synthesis, transition metal chemistry and catalytic studies.
Radhakrishna, Latchupatula; Kunchur, Harish S.; Namdeo, Pavan K.; Butcher, Ray J.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3434–3449; doi:10.1039/c9dt04302k

data_7703165
_publ_section_title
;
 New 1,2,3-triazole based bis- and trisphosphine ligands: synthesis,
 transition metal chemistry and catalytic studies.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3434
_journal_page_last               3449
_journal_paper_doi               10.1039/c9dt04302k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C38 H29 Cl2 N3 P2 Pd, 1(C H2 Cl2)'
_chemical_formula_sum            'C39 H31 Cl4 N3 P2 Pd'
_chemical_formula_weight         851.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-25 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5130(2)
_cell_length_b                   13.1004(2)
_cell_length_c                   25.2960(4)
_cell_measurement_reflns_used    62576
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2820
_cell_measurement_theta_min      2.1440
_cell_volume                     3715.07(11)
_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 0.945
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            98012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.180
_diffrn_reflns_theta_min         2.391
_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    0.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84201
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         11376
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0285P)^2^+2.3111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10690
_reflns_number_total             11376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04302k2.cif
_cod_data_source_block           compound-14
_cod_depositor_comments
'Adding full bibliography for 7703162--7703172.cif.'
_cod_database_code               7703165
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1S-Cl11 = C1S-Cl12
 1.76701 with sigma of 0.02
 C1T-Cl21 = C1T-Cl22
 1.76701 with sigma of 0.02
 C1U-Cl31 = C1U-Cl32
 1.76701 with sigma of 0.02
 Cl11-Cl12 = Cl21-Cl22 = Cl31-Cl32
 2.885527 with sigma of 0.02
3. Rigid bond restraints
 C33, C34, C35, C36, C37, C38, C33A, C34A, C35A, C36A, C37A, C38A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl11, Cl12, C1T, Cl21, Cl22, C1U, Cl31, Cl32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C33A \\sim C34A
\\sim C35A \\sim C36A \\sim C37A \\sim C38A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Cl11 \\sim Cl12 \\sim C1T \\sim Cl21 \\sim Cl22 \\sim C1U \\sim Cl31 \\sim
Cl32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 1*[Sof(C1S)+Sof(H1SA)+Sof(H1SB)+Sof(Cl11)+Sof(Cl12)]+1*[Sof(C1T)+Sof(H1TA)+
 Sof(H1TB)+Sof(Cl21)+Sof(Cl22)]+1*[Sof(C1U)+Sof(H1UA)+Sof(H1UB)+Sof(Cl31)+
 Sof(Cl32)]=1 with esd of 0.0001
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1.633*FVAR(2)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(Cl11)=Sof(Cl12)=FVAR(2)
 Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(Cl21)=Sof(Cl22)=FVAR(3)
 Sof(C1U)=Sof(H1UA)=Sof(H1UB)=Sof(Cl31)=Sof(Cl32)=FVAR(4)
 Sof(C33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=1-FVAR(5)
 Sof(C33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=
 Sof(H37)=Sof(C38)=Sof(H38)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1T(H1TA,H1TB), C1U(H1UA,H1UB)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C2(H2), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C34A(H34A),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A)
6.c Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38), C33A(C34A,C35A,C36A,C37A,C38A)
;
_shelx_res_checksum              41807
_olex2_submission_special_instructions 'No special instructions were received'