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_7716164
_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 Se Zn'
_chemical_formula_sum            'C31 H47 N4 P Se Zn'
_chemical_formula_weight         650.26
_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                 105.609(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0079(4)
_cell_length_b                   16.5327(4)
_cell_length_c                   18.6878(6)
_cell_measurement_reflns_used    9554
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.8630
_cell_measurement_theta_min      2.7120
_cell_volume                     3275.57(19)
_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-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_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     51.00  92.00   0.50   85.22    --    7.10  77.00-150.00   82
  2  \w     62.00  96.00   0.50   85.22    --    7.10  77.00 -30.00   68
  3  \w    -52.00  10.00   0.50   85.22    --   -7.50 -82.00 150.00  124
  4  \w    -21.00  35.00   0.50   85.22    --   -7.50 -82.00  30.00  112
  5  \w    -60.00 -31.00   0.50   85.22    --   -7.50 -82.00  30.00   58
  6  \w    -37.00  36.00   0.50   85.22    --   -7.50  57.00 -90.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085854000
_diffrn_orient_matrix_UB_12      0.0424842000
_diffrn_orient_matrix_UB_13      -0.0033669000
_diffrn_orient_matrix_UB_21      -0.0613102000
_diffrn_orient_matrix_UB_22      -0.0059453000
_diffrn_orient_matrix_UB_23      -0.0239454000
_diffrn_orient_matrix_UB_31      -0.0253420000
_diffrn_orient_matrix_UB_32      0.0000158000
_diffrn_orient_matrix_UB_33      0.0311238000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26776
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.911
_diffrn_reflns_theta_min         2.711
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             1358.7
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0388P)^2^+2.6476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5458
_reflns_number_total             7524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00840e2.cif
_cod_data_source_block           aj1937
_cod_depositor_comments
'Adding full bibliography for 7716164--7716167.cif.'
_cod_database_code               7716164
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N P Se Zn'
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.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)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), 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)
;
_shelx_res_checksum              49138
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.537