N^N <i>vs.</i> N^E (E = S or Se) coordination behavior of imino-phosphanamidinate chalcogenide ligands towards aluminum alkyls: efficient hydroboration catalysis of nitriles, alkynes, and alkenes.
Karmakar, Himadri; Kumar, Ravi; Sharma, Jyoti; Bag, Jayanta; Pal, Kuntal; Panda, Tarun K.; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00038a

data_7712641
_publ_section_title
;
 N^N <i>vs.</i> N^E (E = S or Se) coordination behavior of
 imino-phosphanamidinate chalcogenide ligands towards aluminum alkyls:
 efficient hydroboration catalysis of nitriles, alkynes, and alkenes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00038a
_journal_year                    2023
_chemical_formula_moiety         'C39 H47 N4 P S'
_chemical_formula_sum            'C39 H47 N4 P S'
_chemical_formula_weight         634.83
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                94.52(3)
_cell_angle_beta                 100.34(2)
_cell_angle_gamma                105.00(3)
_cell_formula_units_Z            2
_cell_length_a                   8.446(6)
_cell_length_b                   12.251(9)
_cell_length_c                   18.836(15)
_cell_measurement_reflns_used    27080
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.102
_cell_measurement_theta_min      2.180
_cell_volume                     1836(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27080
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.180
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0842P)^2^+0.5639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4701
_reflns_number_total             7717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00038a2.cif
_cod_data_source_block           3a
_cod_database_code               7712641
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C15) = Uanis(C42)
Uanis(C41) = Uanis(C13) = Uanis(C40)
3. Others
 Fixed Sof: H10(0.5) H10A(0.5) H11(0.5) H11A(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C40(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C10(H10A), C11(H11), C11(H11A)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C20(H20), C27(H27),
 C29(H29), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              61882
_olex2_submission_special_instructions 'No special instructions were received'