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_4519077
_publ_section_title
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 New Volatile Tantalum Imido Precursors with Carboxamide Ligands
;
_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         'C25 H50 N4 O6 Ta'
_chemical_formula_sum            'C25 H50 N4 O6 Ta'
_chemical_formula_weight         683.64
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6888(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4733(3)
_cell_length_b                   16.5773(4)
_cell_length_c                   17.1424(4)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.73
_cell_volume                     3244.36(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9932
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.9956
_diffrn_reflns_Laue_measured_fraction_max 0.9932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43467
_diffrn_reflns_point_group_measured_fraction_full 0.9956
_diffrn_reflns_point_group_measured_fraction_max 0.9932
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.427
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4625
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1268 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.6206.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396.0
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.4901
_refine_diff_density_min         -3.2538
_refine_diff_density_rms         0.2742
_refine_ls_d_res_high            0.8271
_refine_ls_d_res_low             11.8882
_refine_ls_goodness_of_fit_ref   1.1031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    92
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.0952
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+52.5149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -10
_reflns_number_gt                4676
_reflns_number_total             6001
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ao1c03659_si_001.cif
_cod_data_source_block           rjy03-2
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4519077
_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
 C55-C17 \\sim C17-C2
 with sigma of 0.02
3. Rigid bond restraints
 C55, C17, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C55 \\sim C17 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Uanis(C55) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C28(0.6) H28a(0.6) H28b(0.6) H28c(0.6) C36(0.5) C41(0.5) H41a(0.5)
 H41b(0.5) H41c(0.5) C46(0.5) H46a(0.5) H46b(0.5) H46c(0.5) C55(0.4) H55a(0.4)
 H55b(0.4) H55c(0.4) C1(0.6) H1a(0.6) H1b(0.6) H1c(0.6) C3(0.5) H3a(0.5)
 H3b(0.5) H3c(0.5) C2(0.4) H2a(0.4) H2b(0.4) H2c(0.4) C7(0.6) H7a(0.6) H7b(0.6)
 H7c(0.6) C9(0.5) H9a(0.5) H9b(0.5) H9c(0.5) C8(0.5) H8a(0.5) H8b(0.5) H8c(0.5)
 C12(0.5) H12a(0.5) H12b(0.5) H12c(0.5) C13(0.5) C17(0.4) H17a(0.4) H17b(0.4)
 H17c(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C29(H29a,H29b)
6.b Aromatic/amide H refined with riding coordinates:
 C20(H20)
6.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C26(H26a,H26b,H26c), C28(H28a,H28b,
 H28c), C31(H31a,H31b,H31c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C41(H41a,
 H41b,H41c), C43(H43a,H43b,H43c), C46(H46a,H46b,H46c), C53(H53a,H53b,H53c),
 C55(H55a,H55b,H55c), C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C2(H2a,
 H2b,H2c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C12(H12a,H12b,
 H12c), C17(H17a,H17b,H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'