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_7712638
_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
'C45 H59 N4 P S, 0.25[C6H14], 0.25[C6H14], 0.5[C7H8]'
_chemical_formula_sum            'C51.5 H70 N4 P S'
_chemical_formula_weight         808.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-16
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.15 svn.rb8c1d4dc for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2250(6)
_cell_length_b                   24.0393(10)
_cell_length_c                   25.4474(10)
_cell_measurement_reflns_used    24701
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9650
_cell_measurement_theta_min      2.8450
_cell_volume                     9925.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            133079
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.650
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06282
_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    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10252
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0897P)^2^+1.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7253
_reflns_number_total             10252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00038a2.cif
_cod_data_source_block           2a
_cod_original_formula_sum        'C51.50 H70 N4 P S'
_cod_database_code               7712638
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 \\sim N1-C1A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C1-C6 \\sim C1A-C6A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C2-C7 \\sim C2A-C7A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C2-C9 \\sim C2A-C9A
 with sigma of 0.04
 C3-C7 \\sim C3A-C7A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C6-C10 \\sim C6A-C10A
 with sigma of 0.02
 C6-C11 \\sim C6A-C11A
 with sigma of 0.04
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C7-C9 \\sim C7A-C9A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.04
 C2-C6 \\sim C2A-C6A
 with sigma of 0.04
 C2-C8 \\sim C2A-C8A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.02
 C5-C10 \\sim C5A-C10A
 with sigma of 0.04
 C6-C12 \\sim C6A-C12A
 with sigma of 0.04
 N1-C2 \\sim N1-C2A
 with sigma of 0.04
 C8-C9 \\sim C8A-C9A
 with sigma of 0.04
 N1-C6 \\sim N1-C6A
 with sigma of 0.04
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C1-C5 \\sim C1A-C5A
 with sigma of 0.04
 C1-C7 \\sim C1A-C7A
 with sigma of 0.04
 C1-C10 \\sim C1A-C10A
 with sigma of 0.04
3. Others
 Sof(H1B)=Sof(C1A)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=
 Sof(H3A)=Sof(C2A)=Sof(C7A)=Sof(H7A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H1A)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C22(H22), C25(H25), C34(H34), C37(H37), C7A(H7A), C10A(H10A)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C5A(H5A), C4A(H4A), C3A(H3A)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C12A(H12D,H12E,H12F),
 C11A(H11D,H11E,H11F)
;
_shelx_res_checksum              73386
_shelx_fab_checksum              84581
_platon_squeeze_special_details
;
A solvent mask was calculated and 360 electrons were 
found in a volume of 1742\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 0.5[C6H14] and 0.5[C7H8] per Formula Unit 
which account for 400 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'