Formation of mononuclear N,O-chelate zirconium complexes by direct insertion of epoxide into tetrakis(dimethylamido)zirconium: highly promising approach for developing an ALD precursor of ZrO2 thin films
Jiang, Jianwei; Choi, Sohee; Oh, Jaehyun; Choi, Jihyun; Sun, Ho-Jung; Yoon, Sungho; Dalton Transactions  (2022) –; doi:10.1039/D1DT04207F

data_7709763
_publ_section_title
;
 Formation of mononuclear N,O-chelate zirconium complexes by direct
 insertion of epoxide into tetrakis(dimethylamido)zirconium: highly
 promising approach for developing an ALD precursor of ZrO2 thin films
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04207F
_journal_year                    2022
_chemical_formula_moiety         'C22 H48 N4 O2 Zr'
_chemical_formula_sum            'C22 H48 N4 O2 Zr'
_chemical_formula_weight         491.86
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5782(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9734(3)
_cell_length_b                   9.57200(19)
_cell_length_c                   16.6128(3)
_cell_measurement_reflns_used    20701
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      79.037
_cell_measurement_theta_min      5.327
_cell_volume                     2539.09(8)
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.037
_diffrn_reflns_theta_min         5.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.861
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0519P)^2^+12.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4797
_reflns_number_total             5328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04207f2.cif
_cod_data_source_block           ysh-j-1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7709763
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.824
_shelxl_version_number           2013-4
_shelx_res_checksum              5699