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_7703167
_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         'C42 H29 Mo N3 O4 P2, C2 H3 N'
_chemical_formula_sum            'C44 H32 Mo N4 O4 P2'
_chemical_formula_weight         838.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-16
_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                110.228(4)
_cell_angle_beta                 102.707(4)
_cell_angle_gamma                105.324(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8012(3)
_cell_length_b                   16.0063(7)
_cell_length_c                   16.2933(7)
_cell_measurement_reflns_used    6088
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9240
_cell_measurement_theta_min      2.4300
_cell_volume                     1950.38(18)
_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      150.0
_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 0.890
_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  25.00   0.50   12.00    --  -20.00   0.00 -36.00  270
  2  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00 -36.00  258
  3  \w    -71.00  19.00   0.50   12.00    --  -20.00 -72.00 108.00  180
  4  \w    -49.50   2.00   0.50   12.00    --  -20.00  72.00-108.00  103
  5  \w    -39.00  -9.00   0.50   12.00    --  -20.00 -72.00  36.00   60
  6  \w    -96.00 -88.00   0.50   12.00    --  -20.00   0.00-108.00   16
;
_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  0.1019
_diffrn_reflns_av_unetI/netI     0.1653
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22899
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.202
_diffrn_reflns_theta_min         2.427
_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    0.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72556
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.546
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         11269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.0823
_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^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6742
_reflns_number_total             11269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04302k2.cif
_cod_data_source_block           compound-12
_cod_depositor_comments
'Adding full bibliography for 7703162--7703172.cif.'
_cod_original_cell_volume        1950.37(15)
_cod_database_code               7703167
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.947
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C3(H3), C4(H4), C5(H5), C10(H10), C16(H16), C19(H19),
 C23(H23), C18(H18), C20(H20), C22(H22), C25(H25), C24(H24), C28(H28), C11(H11),
  C17(H17), C26(H26), C34(H34), C12(H12), C30(H30), C38(H38), C13(H13),
 C35(H35), C36(H36), C37(H37), C29(H29), C31(H31), C32(H32)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              48764
_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
;