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_7712644
_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         'C29 H41 N4 P S'
_chemical_formula_sum            'C29 H41 N4 P S'
_chemical_formula_weight         508.69
_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   mixed
_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                90
_cell_angle_beta                 92.918(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8855(6)
_cell_length_b                   15.1007(6)
_cell_length_c                   14.1929(7)
_cell_measurement_reflns_used    43846
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.130
_cell_measurement_theta_min      1.971
_cell_volume                     2972.1(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43812
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_min         1.971
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6564
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0675P)^2^+1.7237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4531
_reflns_number_total             6564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00038a2.cif
_cod_data_source_block           4a
_cod_database_code               7712644
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 N1-H1
 0.96 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C30) = Uanis(C6)
Uanis(C23) = Uanis(C31) = Uanis(C5)
Uanis(C9) = Uanis(C11)
Uanis(C10) = Uanis(C11A)
Uanis(C8) = Uanis(C34)
Uanis(C33) = Uanis(C10A)
Uanis(C19) = Uanis(C32) = Uanis(C7)
4. Rigid body (RIGU) restrains
 C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C8(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10A(0.5) H10A(0.5) C11A(0.5)
 H11A(0.5) H11B(0.5) C34(0.5) C10(0.5) H10B(0.5) H10C(0.5) H10D(0.5) C11(0.5)
 H11C(0.5) H11D(0.5) H11E(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
6.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11A(H11A,H11B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15), C16(H16), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C10A(H10A)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C10(H10B,H10C,H10D), C11(H11C,H11D,
 H11E), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              10240
_olex2_submission_special_instructions 'No special instructions were received'