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_7712647
_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 Se'
_chemical_formula_sum            'C47 H64 Al N4 P Se'
_chemical_formula_weight         821.93
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_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                   10.5605(5)
_cell_length_b                   20.3370(10)
_cell_length_c                   21.8728(9)
_cell_measurement_reflns_used    14919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4380
_cell_measurement_theta_min      2.6900
_cell_volume                     4697.6(4)
_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 1.3 (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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60932
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.923
_diffrn_reflns_theta_min         2.681
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52605
_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    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         11137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0392P)^2^+0.3981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                7994
_reflns_number_total             11137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00038a2.cif
_cod_data_source_block           aj1945
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'UNK' was changed
to 'unk' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7712647
_shelx_shelxl_version_number     2016/6
_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:
 C36(H36), C12(H12), C27(H27), C15(H15), C39(H39), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C32(H32), C10(H10), C47(H47), C33(H33), C34(H34), C43(H43),
 C46(H46), C20(H20), C45(H45), C9(H9), C22(H22), C8(H8), C21(H21), C44(H44)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C28(H28A,H28B,H28C),
 C37(H37A,H37B,H37C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C16(H16A,H16B,H16C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C40(H40A,
 H40B,H40C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              5600
_olex2_submission_special_instructions 'No special instructions were received'