Chalcogenoether complexes of Nb(V) thio- and seleno-halides as single source precursors for low pressure chemical vapour deposition of NbS2 and NbSe2 thin films
Chang, Yao-Pang; Hector, Andrew L.; Levason, William; Reid, Gillian; Dalton Trans.  (2017) –; doi:10.1039/C7DT01911D

data_7043429
_publ_section_title
;
 Chalcogenoether complexes of Nb(V) thio- and seleno-halides as single
 source precursors for low pressure chemical vapour deposition of NbS2 and
 NbSe2 thin films
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01911D
_journal_year                    2017
_chemical_formula_moiety         'C4 H10 Cl3 Nb S3'
_chemical_formula_sum            'C4 H10 Cl3 Nb S3'
_chemical_formula_weight         353.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-07 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.502(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2010(3)
_cell_length_b                   11.3494(4)
_cell_length_c                   7.8693(5)
_cell_measurement_reflns_used    4775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2020
_cell_measurement_theta_min      2.8360
_cell_volume                     580.47(6)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5010
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       Chip
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
; 
 Flack x determined using 1010 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2251
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0226P)^2^+0.2849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                2212
_reflns_number_total             2251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01911d2.cif
_cod_data_source_block           2016_0505r2
_cod_database_code               7043429
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              20409