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_7032614
_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         'Cl6 Ta, C7 H15 Te2'
_chemical_formula_sum            'C7 H15 Cl6 Ta Te2'
_chemical_formula_weight         748.07
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.217(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.433(1)
_cell_length_b                   9.1611(12)
_cell_length_c                   25.663(3)
_cell_measurement_reflns_used    6499
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     1747.5(4)
_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  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9189
_diffrn_measured_fraction_theta_max 0.9189
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -107.0000 - 73.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: -120.0000
                 XTD: 45.0000
              2theta: -17.0000
scan:
    Number of images: 31
               Slice: -71.0000 - -40.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -150.0000
                 XTD: 45.0000
              2theta: -17.0000
scan:
    Number of images: 87
               Slice: -107.0000 - -20.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: -150.0000
                 XTD: 45.0000
              2theta: -17.0000
;
_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 50um'
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.073260
_diffrn_orient_matrix_UB_12      -0.023161
_diffrn_orient_matrix_UB_13      -0.031700
_diffrn_orient_matrix_UB_21      0.040243
_diffrn_orient_matrix_UB_22      -0.104025
_diffrn_orient_matrix_UB_23      0.001932
_diffrn_orient_matrix_UB_31      -0.105420
_diffrn_orient_matrix_UB_32      -0.023615
_diffrn_orient_matrix_UB_33      0.022579
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.2056
_diffrn_reflns_av_unetI/netI     0.2260
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11709
_diffrn_reflns_theta_full        25.9994
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_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    10.455
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_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_colour_primary    orange
_exptl_crystal_density_diffrn    2.8432
_exptl_crystal_description       plate
_exptl_crystal_F_000             1342.5254
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         4.9476
_refine_diff_density_min         -4.8853
_refine_diff_density_rms         1.1828
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.4423
_refine_ls_goodness_of_fit_ref   1.0588
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3163
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.0449
_refine_ls_R_factor_all          0.2054
_refine_ls_R_factor_gt           0.1048
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+50.1550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2439
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                1564
_reflns_number_total             3163
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4dt02694b2.cif
_cod_data_source_block           2014slbRmlh2b
_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               7032614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C6, C4, C7, C5, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C4 \\sim C7 \\sim C5 \\sim C1 \\sim C2 \\sim C3: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b)
4.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C7(H7a,H7b,H7c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'