Hydroboration of carbon dioxide enabled by molecular zinc dihydrides.
Wang, Xiaoming; Chang, Kejian; Xu, Xin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7324–7327; doi:10.1039/d0dt01090a

data_7704523
_publ_section_title
;
 Hydroboration of carbon dioxide enabled by molecular zinc dihydrides.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7324
_journal_page_last               7327
_journal_paper_doi               10.1039/d0dt01090a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H61 N2 O2 P Zn'
_chemical_formula_sum            'C50 H61 N2 O2 P Zn'
_chemical_formula_weight         818.34
_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
_audit_creation_date             2019-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-30 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.462(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0915(10)
_cell_length_b                   10.6678(4)
_cell_length_c                   40.3216(18)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.72
_cell_volume                     8784.9(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            142705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         1.979
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0917 before and 0.0648 after correction. The Ratio of minimum to maximum transmission is 0.8479. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.061
_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     1060
_refine_ls_number_reflns         20209
_refine_ls_number_restraints     2284
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0307P)^2^+7.5983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15241
_reflns_number_total             20209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01090a2.cif
_cod_data_source_block           Complex_2b
_cod_depositor_comments
'Adding full bibliography for 7704522--7704523.cif.'
_cod_database_code               7704523
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.842
_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
 C83B-C84B = C83B-C85B
 0.02 with sigma of 1.52
 C83A-C84A = C83A-C85A
 0.02 with sigma of 1.52
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92
\\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim
C100 \\sim C83A \\sim C84A \\sim C83B \\sim C85B \\sim C85A \\sim C84B: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C83A(0.5) H83A(0.5) C84A(0.5) H84A(0.5) H84B(0.5) H84C(0.5)
 C83B(0.5) H83B(0.5) C85B(0.5) H85A(0.5) H85B(0.5) H85C(0.5) C85A(0.5)
 H85D(0.5) H85E(0.5) H85F(0.5) C84B(0.5) H84D(0.5) H84E(0.5) H84F(0.5)
5.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C45(H45), C48(H48), C86(H86), C95(H95), C98(H98),
 C83A(H83A), C83B(H83B)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C63(H63A,H63B), C64(H64A,H64B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C41(H41), C42(H42), C43(H43), C52(H52), C53(H53), C56(H56),
 C58(H58), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C79(H79), C80(H80), C81(H81), C91(H91),
 C92(H92), C93(H93)
5.d Idealised Me refined as rotating group:
 C10(H10D,H10E,H10F), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C99(H99A,
 H99B,H99C), C100(H10A,H10B,H10C), C84A(H84A,H84B,H84C), C85B(H85A,H85B,H85C),
 C85A(H85D,H85E,H85F), C84B(H84D,H84E,H84F)
;
_shelx_res_checksum              9100
_olex2_submission_special_instructions 'No special instructions were received'