Tri-coordinated zinc alkyl complexes with <i>N</i>^<i>S</i>/<i>Se</i> coordination of imino-phosphanamidinate chalcogenide ligands as precursors for efficient hydroboration of nitriles and esters.
Karmakar, Himadri; Kumar, Gobbilla Sai; Pal, Kuntal; Chandrasekhar, Vadapalli; Panda, Tarun K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10592–10602; doi:10.1039/d4dt00840e

data_7716165
_publ_section_title
;
 Tri-coordinated zinc alkyl complexes with <i>N</i>^<i>S</i>/<i>Se</i>
 coordination of imino-phosphanamidinate chalcogenide ligands as
 precursors for efficient hydroboration of nitriles and esters.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10592
_journal_page_last               10602
_journal_paper_doi               10.1039/d4dt00840e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H47 N4 P S Zn'
_chemical_formula_sum            'C31 H47 N4 P S Zn'
_chemical_formula_weight         604.15
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-19
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.216(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0220(16)
_cell_length_b                   16.528(3)
_cell_length_c                   18.701(3)
_cell_measurement_reflns_used    33208
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.115
_cell_measurement_theta_min      1.951
_cell_volume                     3287.4(9)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32571
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.115
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+2.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3817
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00840e2.cif
_cod_data_source_block           mo_tkp_hk_lh3szn_0m_a
_cod_depositor_comments
'Adding full bibliography for 7716164--7716167.cif.'
_cod_original_cell_volume        3287.3(8)
_cod_database_code               7716165
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.855
_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
 Zn1A-C1 \\sim Zn1A-C1A
 with sigma of 0.02
 Zn1A-C2 \\sim Zn1A-C2A
 with sigma of 0.04
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C1A) = Uanis(C2) = Uanis(C2A)
4. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C27(H27), C28(H28), C29(H29),
 C30(H30), C31(H31)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C2(H2A,H2B,H2C),
 C2A(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              9337
_olex2_submission_special_instructions 'No special instructions were received'