Niobium(v) and tantalum(v) halide chalcogenoether complexes - towards single source CVD precursors for ME2 thin films.
Benjamin, Sophie L.; Chang, Yao-Pang; Gurnani, Chitra; Hector, Andrew L.; Huggon, Michelle; Levason, William; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16640–16648; doi:10.1039/c4dt02694b

data_7032616
_publ_section_title
;
 Niobium(v) and tantalum(v) halide chalcogenoether complexes - towards
 single source CVD precursors for ME2 thin films.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16640
_journal_page_last               16648
_journal_paper_doi               10.1039/c4dt02694b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C12 H18 Cl10 Nb2 S2'
_chemical_formula_sum            'C12 H18 Cl10 Nb2 S2'
_chemical_formula_weight         766.70
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             13-10-17
_audit_creation_method
;
Rigaku CrystalClear-SM Expert 2.0 r11
;
_cell_angle_alpha                90
_cell_angle_beta                 99.150(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4305(10)
_cell_length_b                   17.5222(10)
_cell_length_c                   11.7030(10)
_cell_measurement_reflns_used    11213
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2516.6(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 128
               Slice: -110.0000 - 18.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 135.0000
                 XTD: 45.0217
              2theta: -19.9971
scan:
    Number of images: 71
               Slice: -110.0000 - -39.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -30.0000
                 Phi: 270.0000
                 XTD: 45.0217
              2theta: -19.9971
scan:
    Number of images: 24
               Slice: -34.0000 - -10.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 90.0000
                 XTD: 45.0217
              2theta: -19.9971
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.016580
_diffrn_orient_matrix_UB_12      -0.055907
_diffrn_orient_matrix_UB_13      0.007350
_diffrn_orient_matrix_UB_21      0.072528
_diffrn_orient_matrix_UB_22      0.011148
_diffrn_orient_matrix_UB_23      0.051847
_diffrn_orient_matrix_UB_31      -0.044222
_diffrn_orient_matrix_UB_32      -0.002677
_diffrn_orient_matrix_UB_33      0.062430
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 0.996
_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         3.216
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+7.2997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4258
_reflns_number_total             4924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02694b2.cif
_cod_data_source_block           ypc2x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032613--7032616.cif.
;
_cod_database_code               7032616
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C11-C12
 with sigma of 0.02
 C10-S2 \\sim C10-S2A
 with sigma of 0.02
 Nb2-Cl7 \\sim Nb2-Cl7A
 with sigma of 0.01
 Nb2-Cl8 \\sim Nb2-Cl8A
 with sigma of 0.01
 Nb2-Cl9 \\sim Nb2-Cl9A
 with sigma of 0.01
 S2-Nb2 \\sim S2A-Nb2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl7A) \\sim Ueq, Uanis(Cl8A) \\sim Ueq, Uanis(Cl9A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl7) = Uanis(Cl7A)
Uanis(Cl8) = Uanis(Cl8A)
Uanis(Cl9) = Uanis(Cl9A)
Uanis(S2) = Uanis(S2A)
4. Others
 Sof(Cl7A)=Sof(Cl8A)=Sof(Cl9A)=Sof(S2A)=Sof(H10C)=Sof(H10D)=Sof(H11C)=
 Sof(H11D)=1-FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(S2)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C10(H10C,H10D), C11(H11A,H11B),
 C11(H11C,H11D)
5.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;