1,2,3-Triazolyl bisphosphine with pyridyl functionality: synthesis, copper(i) chemistry and application in click catalysis
Sheokand, Sonu; Mohite, Manali A.; Mondal, Dipanjan; Rangarajan, Shalini; Balakrishna, Maravanji S.; New Journal of Chemistry 47 (2023) 13538–13546; doi:10.1039/D3NJ01445B

data_7062532
_publ_section_title
;
 1,2,3-Triazolyl bisphosphine with pyridyl functionality: synthesis,
 copper(i) chemistry and application in click catalysis
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13538
_journal_page_last               13546
_journal_paper_doi               10.1039/D3NJ01445B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C38 H31 Br Cu N5 P2, C H2 Cl2'
_chemical_formula_sum            'C39 H33 Br Cl2 Cu N5 P2'
_chemical_formula_weight         847.99
_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
_audit_creation_date             2023-01-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-14 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2611(3)
_cell_length_b                   25.5075(7)
_cell_length_c                   13.8777(4)
_cell_measurement_reflns_used    7137
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.5880
_cell_measurement_theta_min      2.1580
_cell_volume                     3629.68(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -198.27  10.23   0.50    4.00  77.88 -12.98  31.50    --   417
  2  \w   -108.63  15.87   0.50    4.00    --  -12.98 -59.25 -33.92  249
  3  \w   -108.63  15.87   0.50    4.00    --  -12.98 -59.25 -84.92  249
  4  \w   -108.63  15.87   0.50    4.00    --  -12.98 -59.25  20.08  249
  5  \w   -108.63  15.87   0.50    4.00    --  -12.98 -59.25-135.92  249
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63357
_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         2.141
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0368P)^2^+5.4932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5329
_reflns_number_total             6395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01445b2.cif
_cod_data_source_block           comp_3
_cod_depositor_comments
'Adding full bibliography for 7062531--7062533.cif.'
_cod_database_code               7062532
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C19(H19), C4(H4), C38(H38), C25(H25), C9(H9), C21(H21),
 C13(H13), C23(H23), C24(H24), C32(H32), C34(H34), C28(H28), C18(H18), C3(H3),
 C16(H16), C22(H22), C37(H37), C17(H17), C36(H36), C10(H10), C35(H35), C30(H30),
  C12(H12), C31(H31), C29(H29), C11(H11)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              68221
_shelx_hkl_checksum              22868
_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
;