Hexahalometallate salts of trivalent scandium, yttrium and lanthanum: cation‒anion association in the solid state and in solution
Champion, Martin J. D.; Levason, William; Pugh, David; Reid, Gillian; New J. Chem. 40 (2016) 7181–; doi:10.1039/C6NJ01068G

data_7055651
_publ_section_title
;
 Hexahalometallate salts of trivalent scandium, yttrium and lanthanum:
 cation--anion association in the solid state and in solution
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              7181
_journal_paper_doi               10.1039/C6NJ01068G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '3(C7 H13 N2), I6 La'
_chemical_formula_sum            'C21 H39 I6 La N6'
_chemical_formula_weight         1275.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2016-04-06 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                92.594(3)
_cell_angle_beta                 90.255(3)
_cell_angle_gamma                106.930(4)
_cell_formula_units_Z            2
_cell_length_a                   10.347(2)
_cell_length_b                   11.075(3)
_cell_length_c                   16.577(3)
_cell_measurement_reflns_used    5182
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1815.1(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_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
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
    Number of images: 256
               Slice: -110.0000 - 18.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 225.0000
                 XTD: 45.0032
              2theta: -20.0198
scan:
    Number of images: 256
               Slice: -110.0000 - 18.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 0.0000
                 XTD: 45.0032
              2theta: -20.0198
scan:
    Number of images: 132
               Slice: -71.0000 - -5.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -30.0000
                 Phi: 45.0000
                 XTD: 45.0032
              2theta: -20.0198
scan:
    Number of images: 88
               Slice: -90.0000 - -46.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -30.0000
                 Phi: 135.0000
                 XTD: 45.0032
              2theta: -20.0198
scan:
    Number of images: 54
               Slice: -110.0000 - -83.0000
         Image width: 0.5000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -30.0000
                 Phi: 270.0000
                 XTD: 45.0032
              2theta: -20.0198
;
_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 Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.037343
_diffrn_orient_matrix_UB_12      -0.081532
_diffrn_orient_matrix_UB_13      -0.046556
_diffrn_orient_matrix_UB_21      0.088622
_diffrn_orient_matrix_UB_22      0.020874
_diffrn_orient_matrix_UB_23      -0.025297
_diffrn_orient_matrix_UB_31      0.022826
_diffrn_orient_matrix_UB_32      -0.020608
_diffrn_orient_matrix_UB_33      0.051982
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16557
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         2.460
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    6.299
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         8311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7810
_reflns_number_total             8311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01068g1.cif
_cod_data_source_block           2014rmjdc1261x
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055644--7055651.cif.
;
_cod_database_code               7055651
_shelxl_version_number           2014-3
_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.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C11(H11A,H11B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C10(H10), C2(H2), C16(H16), C9(H9), C3(H3)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              64240
_olex2_submission_special_instructions 'No special instructions were received'