Group 3 metal trihalide complexes with neutral N-donor ligands - exploring their affinity towards fluoride.
Curnock, Emily; Levason, William; Light, Mark E.; Luthra, Sajinder K.; McRobbie, Graeme; Monzittu, Francesco M.; Reid, Gillian; Williams, R. Nathan; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6059–6068; doi:10.1039/c8dt00480c

data_7046067
_publ_section_title
;
 Group 3 metal trihalide complexes with neutral N-donor ligands -
 exploring their affinity towards fluoride.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6059
_journal_page_last               6068
_journal_paper_doi               10.1039/c8dt00480c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C12 H30 Cl F3 N3 Sc Sn'
_chemical_formula_sum            'C12 H30 Cl F3 N3 Sc Sn'
_chemical_formula_weight         472.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-27 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.852(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8495(10)
_cell_length_b                   9.2438(6)
_cell_length_c                   10.9099(7)
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3840
_cell_measurement_theta_min      2.1400
_cell_volume                     1046.67(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -113.00 26.00 1.00 10.00 -- -23.00 -18.00 -90.00 139 2 \w -45.00 16.00 1.00 10.00 -- -23.00 -72.00 0.00 61 3 \w -44.00 -8.00 1.00 10.00 -- -23.00 72.00 -90.00 36 4 \w -41.00 -29.00 1.00 10.00 -- -23.00 18.00-180.00 12 5 \w -18.00 -8.00 1.00 10.00 -- -23.00 -54.00-150.00 10 6 \w -62.00 67.00 1.00 10.00 -- -23.00 72.00 30.00 129 7 \w -20.00 53.00 1.00 10.00 -- -23.00 54.00 -90.00 73'
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5546
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         2.131
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                2704
_reflns_number_total             2729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00480c2.cif
_cod_data_source_block           2016fmm7662-54-2r_ml
_cod_depositor_comments
'Adding full bibliography for 7046064--7046071.cif.'
_cod_database_code               7046067
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.732
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1B,H1C,H1A} of C1, {H4AA,H4AB,H4BA} of C4A, All C(H,H)
  groups
 At 1.5 times of:
  {H2AA,H2AB,H2AC} of C2A, {H3AA,H3AB,H3AC} of C3A, {H7A,H7B,H7C} of C7,
  {H3BA,H3BB,H3BC} of C3B, {H2BA,H2BB,H2BC} of C2B
2. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C3B) = Uanis(C3A)
Uanis(F2B) = Uanis(F2A)
Uanis(C2A) = Uanis(C2B)
Uanis(C4B) = Uanis(C4A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F2A(0.5) F2B(0.5) H1B(0.5) H1C(0.5) H1A(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) H2AC(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C3B(0.5) H3BA(0.5)
 H3BB(0.5) H3BC(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4BA(0.5) C4B(0.5) H4BB(0.5)
 C5A(0.5) H5AA(0.5) H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C6A(0.5) H6AA(0.5)
 H6AB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
 C2B(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5)
5.a Riding coordinates:
 C1(H1B,H1C,H1A), C4A(H4AA,H4AB,H4BA), C4B(H4BB)
5.b Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB)
5.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C7(H7A,H7B,
 H7C), C2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              89570
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;