New Volatile Tantalum Imido Precursors with Carboxamide Ligands
Hwang, Jeong Min; Lee, Sung Kwang; Shin, Sunyoung; Jeong, Ji-Seoung; Kim, Hae Sun; Ryu, Ji Yeon; Eom, Taeyong; Park, Bo Keun; Kim, Chang Gyoun; Chung, Taek-Mo; ACS Omega 6 (2021) 24795–24802; doi:10.1021/acsomega.1c03659

data_4519076
_publ_section_title
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 New Volatile Tantalum Imido Precursors with Carboxamide Ligands
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_journal_issue                   38
_journal_name_full               'ACS Omega'
_journal_page_first              24795
_journal_page_last               24802
_journal_paper_doi               10.1021/acsomega.1c03659
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C22 H48 N4 O6 Ta'
_chemical_formula_sum            'C22 H48 N4 O6 Ta'
_chemical_formula_weight         645.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2677(2)
_cell_length_b                   16.0705(2)
_cell_length_c                   11.2870(2)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      3.56
_cell_volume                     2950.76(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9950
_diffrn_measured_fraction_theta_max 0.9946
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.9950
_diffrn_reflns_Laue_measured_fraction_max 0.9946
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38808
_diffrn_reflns_point_group_measured_fraction_full 0.9950
_diffrn_reflns_point_group_measured_fraction_max 0.9946
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0942 before and 0.0396 after correction.
The Ratio of minimum to maximum transmission is 0.7401.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1316.0
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.3736
_refine_diff_density_min         -0.5428
_refine_diff_density_rms         0.0865
_refine_ls_d_res_high            0.8168
_refine_ls_d_res_low             5.0605
_refine_ls_goodness_of_fit_ref   1.0435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0435
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.9922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2708
_reflns_number_total             2920
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ao1c03659_si_002.cif
_cod_data_source_block           RJY01-1
_cod_database_code               4519076
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H10a(0.5) H10b(0.5) H10c(0.5) H3a(0.5) H3b(0.5) H3c(0.5)
3.a Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C3(H3a,H3b,
 H3c), C2(H2a,H2b,H2c), C9(H9a,H9b,H9c), C4(H4a,H4b,H4c), C8(H8a,H8b,H8c),
 C7(H7a,H7b,H7c)
;
_olex2_submission_special_instructions 'No special instructions were received'