Zinc hydride catalyzed hydroboration of esters.
Patro, A. Ganesh; Sahoo, Rajata Kumar; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3621–3628; doi:10.1039/d3dt04084d

data_7715352
_publ_section_title
;
 Zinc hydride catalyzed hydroboration of esters.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3621
_journal_page_last               3628
_journal_paper_doi               10.1039/d3dt04084d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C98 H122 N10 O2 Zn2'
_chemical_formula_sum            'C98 H122 N10 O2 Zn2'
_chemical_formula_weight         1602.79
_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     dual
_audit_creation_date             2023-02-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-03-02 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.62480(10)
_cell_length_b                   14.65430(10)
_cell_length_c                   19.2404(2)
_cell_measurement_reflns_used    28439
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1780
_cell_measurement_theta_min      4.0080
_cell_volume                     4340.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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   -102.00 -31.00   0.50    1.11    --  -38.50 -51.00 169.00  142
  2  \w    -45.00  25.00   0.50    1.11    --  -38.50  51.00 -44.00  140
  3  \w     43.00 113.00   0.50    1.11    --   49.56  51.00 -44.00  140
  4  \w    -14.00  57.00   0.50    1.11    --   49.56 -51.00 169.00  142
  5  \w     39.00 110.00   0.50    2.62    --  102.63 -51.00 169.00  142
  6  \w     96.00 166.00   0.50    2.62    --  102.63  51.00 -44.00  140
  7  \w    -86.00  -6.00   0.50    1.11    --  -38.50 125.00  30.00  160
  8  \w     28.00 101.00   0.50    1.11    --   49.56-125.00-180.00  146
  9  \w     38.00 112.00   0.50    2.62    --  102.63-125.00-180.00  148
 10  \w     40.00 116.00   0.50    2.62    --  102.63 -61.00-120.00  152
 11  \w     38.00 126.00   0.50    2.62    --  102.63 -77.00  90.00  176
 12  \w     34.00 107.00   0.50    2.62    --  102.63 -94.00  60.00  146
 13  \w    103.00 167.00   0.50    2.62    --  102.63  77.00-180.00  128
 14  \w     40.00 116.00   0.50    2.62    --  102.63 -61.00 120.00  152
 15  \w     38.00 107.00   0.50    2.62    --  102.63 -45.00 -90.00  138
 16  \w     98.00 167.00   0.50    2.62    --  102.63  45.00-150.00  138
 17  \w    103.00 167.00   0.50    2.62    --  102.63  77.00 -30.00  128
 18  \w     97.00 168.00   0.50    2.62    --  102.63 125.00 150.00  142
 19  \w     38.00 113.00   0.50    1.11    --   49.56  57.00  60.00  150
;
_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      -0.0625452000
_diffrn_orient_matrix_UB_12      -0.0798312000
_diffrn_orient_matrix_UB_13      -0.0234282000
_diffrn_orient_matrix_UB_21      -0.0631682000
_diffrn_orient_matrix_UB_22      0.0661318000
_diffrn_orient_matrix_UB_23      -0.0451528000
_diffrn_orient_matrix_UB_31      0.0460238000
_diffrn_orient_matrix_UB_32      -0.0177614000
_diffrn_orient_matrix_UB_33      -0.0633324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.699
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
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    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0600P)^2^+13.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8530
_reflns_number_total             8828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04084d2.cif
_cod_data_source_block           sn-agp-c2-65_auto
_cod_database_code               7715352
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Zn'
_diffrn_oxdiff_digest_frames
;
01ef7443a7a3601a23800100b80fa0bb1800027c666
;
_diffrn_oxdiff_digest_hkl
;
014498c27301fd42308d2961a0975b063a713b
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 O1, C003
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C01K, C01J
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C01D, C00Q
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C003) = Uanis(C00Q)
4.a Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B), C00W(H00F,H00G), C00Y(H00I,H00J), C015(H01A,H01B), C017(H01C,
 H01D), C018(H01E,H01F), C01A(H01J,H01K), C01J(H0AA,HF)
4.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C00C(H00C), C00D(H00D), C00E(H00E), C00H(H00H), C00P(H00P),
 C00Q(H00Q), C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C016(H016), C01E(H01U)
4.c Idealised Me refined as rotating group:
 C019(H01G,H01H,H01I), C01B(H01L,H01M,H01N), C01C(H01O,H01P,H01Q), C01D(H01R,
 H01S,H01T), C01F(H01V,H01W,H01X), C01G(H01Y,H,HA), C01H(H01Z,HB,HC), C01I(H01,
 HD,HE), C01K(H1AA,HG,HH)
;
_shelx_res_checksum              87208
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.530