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_7712648
_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_absolute_configuration unk
_chemical_formula_moiety         'C47 H64 Al N4 P S'
_chemical_formula_sum            'C47 H64 Al N4 P S'
_chemical_formula_weight         775.080
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_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            4
_cell_length_a                   10.6056(4)
_cell_length_b                   20.2557(7)
_cell_length_c                   21.7565(7)
_cell_measurement_reflns_used    13696
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      27.0330
_cell_measurement_theta_min      2.8550
_cell_volume                     4673.8(3)
_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  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44544
_diffrn_reflns_point_group_measured_fraction_full 0.9953
_diffrn_reflns_point_group_measured_fraction_max 0.9848
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70905
_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    1.101
_exptl_crystal_description       block
_exptl_crystal_F_000             1673.925
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.2044
_refine_diff_density_min         -0.2470
_refine_diff_density_rms         0.0397
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_d_res_high            0.7829
_refine_ls_d_res_low             7.5939
_refine_ls_goodness_of_fit_ref   1.0220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     501
_refine_ls_number_reflns         10061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0220
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.4247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.971
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                8465
_reflns_number_total             10061
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00038a2.cif
_cod_data_source_block           5a
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7712648
_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 Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C15(H15), C12(H12), C36(H36), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C21(H21), C20(H20), C22(H22), C47(H47), C43(H43), C10(H10),
 C34(H34), C45(H45), C9(H9), C8(H8), C46(H46), C44(H44), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C4(H4a,H4b,H4c), C14(H14a,H14b,H14c), C25(H25a,H25b,H25c),
 C13(H13a,H13b,H13c), C17(H17a,H17b,H17c), C37(H37a,H37b,H37c), C38(H38a,H38b,
 H38c), C28(H28a,H28b,H28c), C26(H26a,H26b,H26c), C29(H29a,H29b,H29c), C16(H16a,
 H16b,H16c), C41(H41a,H41b,H41c), C40(H40a,H40b,H40c)
;
_olex2_submission_special_instructions 'No special instructions were received'