Synthesis of low oxidation state zinc(i) complexes and their catalytic studies in the dehydroborylation of terminal alkynes
Sahoo, Rajata Kumar; Rajput, Sagrika; Patro, A. Ganesh; Nembenna, Sharanappa; Dalton Transactions  (2022) –; doi:10.1039/D2DT02846H

data_7711444
_publ_section_title
;
 Synthesis of low oxidation state zinc(i) complexes and their catalytic
 studies in the dehydroborylation of terminal alkynes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02846H
_journal_year                    2022
_chemical_formula_moiety         'C102 H122 N10 Zn2'
_chemical_formula_sum            'C102 H122 N10 Zn2'
_chemical_formula_weight         1618.83
_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     direct
_audit_creation_date             2022-07-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2022-07-29 deposited with the CCDC.	2022-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                77.6300(10)
_cell_angle_beta                 71.4150(10)
_cell_angle_gamma                71.6870(10)
_cell_formula_units_Z            1
_cell_length_a                   12.89300(10)
_cell_length_b                   12.9295(2)
_cell_length_c                   14.8009(2)
_cell_measurement_reflns_used    26167
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.8960
_cell_measurement_theta_min      3.4820
_cell_volume                     2202.29(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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      1.00  71.00   0.50   17.93    --    4.39  36.00 105.00  140
  2  \w    -62.00   8.00   0.50   17.93    --    4.39 -36.00 -51.00  140
  3  \w    -72.00  -2.00   0.50   17.93    --   -5.01 -36.00 -51.00  140
  4  \w     -8.00  45.00   0.50   17.93    --   -5.01  36.00 105.00  106
  5  \w      2.00  68.00   0.50   17.93    --    4.39  37.00-120.00  132
  6  \w    -41.00  18.00   0.50   17.93    --   -5.01 -77.00  90.00  118
  7  \w    -41.00   2.00   0.50   17.93    --   -5.01 -77.00   0.00   86
  8  \w    -42.00  16.00   0.50   17.93    --   -5.01 -77.00-120.00  116
  9  \w      1.00  59.00   0.50   17.93    --   -5.01  19.00 -30.00  116
 10  \w    -33.00  -6.00   0.50   17.93    --   -5.01 -57.00 -60.00   54
 11  \w    -10.00  31.00   0.50   17.93    --   -5.01 -99.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0515908000
_diffrn_orient_matrix_UB_12      0.0375124000
_diffrn_orient_matrix_UB_13      0.0207901000
_diffrn_orient_matrix_UB_21      0.0309817000
_diffrn_orient_matrix_UB_22      0.0305727000
_diffrn_orient_matrix_UB_23      0.0103179000
_diffrn_orient_matrix_UB_31      0.0017408000
_diffrn_orient_matrix_UB_32      0.0324324000
_diffrn_orient_matrix_UB_33      -0.0453796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38471
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0499P)^2^+1.4111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8119
_reflns_number_total             8979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02846h2.cif
_cod_data_source_block           sn_rks_c9_71
_cod_database_code               7711444
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C102 H120 N10 Zn2 '
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.890
_diffrn_oxdiff_digest_frames
;
01a8dd2307e9d9446b385163c5233e977100025621e
;
_diffrn_oxdiff_digest_hkl
;
012ff3d4d10a951afb68e4fe2c06b79cb26c48
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C49)
3.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C23(H23A,H23B), C21(H21A,H21B), C37(H37A,H37B), C35(H35A,
 H35B), C47(H47A,H47B), C45(H45A,H45B), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C19(H19), C17(H17), C5(H5A), C6(H6), C4(H4A), C18(H18),
 C33(H33), C32(H32), C53(H53), C54(H54), C43(H43), C50(H50), C41(H41), C42(H42),
  C31(H31), C51(H51)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C36(H36A,H36B,
 H36C), C57(H57A,H57B,H57C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C38(H38A,
 H38B,H38C), C26(H26A,H26B,H26C)
;
_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 1.657
_oxdiff_exptl_absorpt_empirical_full_min 0.592