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_7716166
_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         'C47 H63 N4 P Se Zn'
_chemical_formula_sum            'C47 H63 N4 P Se Zn'
_chemical_formula_weight         859.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 101.243(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6029(4)
_cell_length_b                   38.6821(18)
_cell_length_c                   12.2040(5)
_cell_measurement_reflns_used    14792
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.0960
_cell_measurement_theta_min      2.7270
_cell_volume                     4446.3(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 1.3-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 0.990
_diffrn_measured_fraction_theta_max 0.859
_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    -46.00 -21.00   0.25    8.54    --    7.10 -59.00 -21.00  100
  2  \w     12.00  37.00   0.25    8.54    --    7.10  59.00 119.00  100
  3  \w    -46.00 -21.00   0.25    8.54    --   -7.50 -59.00 -21.00  100
  4  \w     -3.00  22.00   0.25    8.54    --   -7.50  59.00 119.00  100
  5  \w     55.00  94.00   0.25    8.54    --    7.10  77.00-180.00  156
  6  \w     53.00  78.00   0.25    8.54    --    7.10  77.00 -30.00  100
  7  \w     54.00  81.00   0.25    8.54    --    7.10  77.00   0.00  108
  8  \w     69.00  96.00   0.25    8.54    --    7.10  77.00  60.00  108
  9  \w    -63.00  -1.00   0.25    8.54    --   -7.50 -82.00 120.00  248
 10  \w    -94.00  15.00   0.25    8.54    --   -7.50 -57.00 -90.00  436
;
_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      -0.0510251000
_diffrn_orient_matrix_UB_12      0.0084139000
_diffrn_orient_matrix_UB_13      0.0256366000
_diffrn_orient_matrix_UB_21      -0.0242521000
_diffrn_orient_matrix_UB_22      0.0094737000
_diffrn_orient_matrix_UB_23      -0.0497470000
_diffrn_orient_matrix_UB_31      -0.0497499000
_diffrn_orient_matrix_UB_32      -0.0132569000
_diffrn_orient_matrix_UB_33      -0.0195404000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45472
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.946
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27304
_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    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         10081
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2.3940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6909
_reflns_number_total             10081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00840e2.cif
_cod_data_source_block           aj1936
_cod_depositor_comments
'Adding full bibliography for 7716164--7716167.cif.'
_cod_database_code               7716166
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNSePZn
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.680
_reflns_odcompleteness_completeness 98.29
_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. Restrained distances
 Zn1-C2 \\sim Zn1-C2A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) = Uanis(C2) = Uanis(C1) = Uanis(C2A) = Uanis(C1A)
4. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C25(H25), C27(H27), C36(H36), C39(H39)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB)
5.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
 C32(H32), C33(H33), C34(H34), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
5.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C)
;
_shelx_res_checksum              99477
_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 3.329
_oxdiff_exptl_absorpt_empirical_full_min 0.647