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_7716167
_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 S Zn, 1(C7 H8)'
_chemical_formula_sum            'C54 H71 N4 P S Zn'
_chemical_formula_weight         904.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                94.294(2)
_cell_angle_beta                 97.700(2)
_cell_angle_gamma                109.859(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4591(2)
_cell_length_b                   13.2462(3)
_cell_length_c                   22.8703(6)
_cell_measurement_reflns_used    18586
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.9710
_cell_measurement_theta_min      2.8410
_cell_volume                     2648.49(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.899
_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     59.00  84.00   0.50   13.07    --   10.80  79.00  31.00   50
  2  \w    -33.00  -8.00   0.50   13.07    --   10.80 -79.00 -92.00   50
  3  \w    -52.00  -9.00   0.50   13.07    --  -11.40 -79.00 -92.00   86
  4  \w     50.00  95.00   0.50   13.07    --   10.80  77.00-120.00   90
  5  \w     49.00 100.00   0.50   13.07    --   10.80  77.00-180.00  102
  6  \w     26.00  51.00   0.50   13.07    --   10.80 -38.00 120.00   50
  7  \w    -79.00  20.00   0.50   13.07    --   10.80 -38.00 120.00  198
  8  \w    -59.00  26.00   0.50   13.07    --  -11.40 -82.00 -30.00  170
  9  \w    -64.00   1.00   0.50   13.07    --  -11.40 -82.00   0.00  130
 10  \w    -19.00   8.00   0.50   13.07    --  -11.40 -38.00  60.00   54
 11  \w    -64.00   2.00   0.50   13.07    --  -11.40 -82.00-150.00  132
 12  \w   -101.00 -49.00   0.50   13.07    --  -11.40 -38.00  60.00  104
 13  \w    -53.00  31.00   0.50   13.07    --  -11.40  38.00-180.00  168
 14  \w    -44.00 -19.00   0.50   13.07    --  -11.40 -82.00  90.00   50
;
_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      -0.0424552000
_diffrn_orient_matrix_UB_12      -0.0420091000
_diffrn_orient_matrix_UB_13      -0.0233898000
_diffrn_orient_matrix_UB_21      0.0319954000
_diffrn_orient_matrix_UB_22      -0.0355512000
_diffrn_orient_matrix_UB_23      0.0135616000
_diffrn_orient_matrix_UB_31      -0.0609866000
_diffrn_orient_matrix_UB_32      -0.0163633000
_diffrn_orient_matrix_UB_33      0.0162809000
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54508
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.584
_diffrn_reflns_theta_min         2.428
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90382
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         14650
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0749P)^2^+2.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10496
_reflns_number_total             14650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00840e2.cif
_cod_data_source_block           aj2209
_cod_depositor_comments
'Adding full bibliography for 7716164--7716167.cif.'
_cod_original_cell_volume        2648.49(11)
_cod_database_code               7716167
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNPSZn
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C51-C52 \\sim C51A-C52A
 with sigma of 0.02
 C54-C50A \\sim C54A-C50B
 with sigma of 0.04
 C52-C54 \\sim C52A-C54A
 with sigma of 0.04
 C51-C54 \\sim C51A-C54A
 with sigma of 0.02
 C51-C50A \\sim C51A-C50B
 with sigma of 0.02
 C52-C50A \\sim C52A-C50B
 with sigma of 0.04
 C48-C50A \\sim C48A-C50B
 with sigma of 0.04
 C52-C53 \\sim C52A-C53A
 with sigma of 0.02
 C52-C48 \\sim C52A-C48A
 with sigma of 0.04
 C48-C53 \\sim C48A-C53A
 with sigma of 0.02
 C48-C49A \\sim C48A-C49B
 with sigma of 0.02
 C50A-C49A \\sim C50B-C49B
 with sigma of 0.02
 C53-C49A \\sim C53A-C49B
 with sigma of 0.04
 C51-C53 \\sim C51A-C53A
 with sigma of 0.04
 C51-C49A \\sim C51A-C49B
 with sigma of 0.04
3. Restrained planarity
 C48A, C53A, C52A, C51A, C49B, C50B
 with sigma of 0.1
 C51, C52, C48, C53, C50A, C49A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C52) = Uanis(C48) = Uanis(C53) = Uanis(C50A) = Uanis(C49A) =
Uanis(C48A) = Uanis(C53A) = Uanis(C52A) = Uanis(C51A) = Uanis(C49B) =
Uanis(C50B)
Uanis(C54A) = Uanis(C54)
5. Others
 Sof(C48A)=Sof(H48A)=Sof(C53A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=Sof(C51A)=
 Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C49B)=Sof(H49B)=Sof(C50B)=
 Sof(H50B)=1-FVAR(1)
 Sof(C51)=Sof(C52)=Sof(H52)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C48)=
 Sof(H48)=Sof(C53)=Sof(H53)=Sof(C50A)=Sof(H50A)=Sof(C49A)=Sof(H49A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C39(H39), C9(H9), C27(H27), C24(H24), C36(H36)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C32(H32), C34(H34), C47(H47), C33(H33), C22(H22),
 C43(H43), C20(H20), C5(H5), C21(H21), C46(H46), C7(H7), C6(H6), C45(H45),
 C44(H44), C52(H52), C48(H48), C53(H53), C50A(H50A), C49A(H49A), C48A(H48A),
 C53A(H53A), C52A(H52A), C49B(H49B), C50B(H50B)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C29(H29A,H29B,H29C), C11(H11A,H11B,H11C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C),
 C2(H2A,H2B,H2C), C54(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27018
_shelx_fab_checksum              10935
_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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.862