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_7046068
_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         'C9 H21 Cl F2 N3 Sc'
_chemical_formula_sum            'C9 H21 Cl F2 N3 Sc'
_chemical_formula_weight         289.70
_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     direct
_audit_creation_date             2017-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.292(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9938(9)
_cell_length_b                   6.8826(7)
_cell_length_c                   15.8721(19)
_cell_measurement_reflns_used    2643
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.7050
_cell_measurement_theta_min      2.5930
_cell_volume                     1310.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -84.00  36.00   1.00   10.00    --  -23.00  18.00 -90.00  120
  2  \w    -59.00  67.00   1.00   10.00    --  -23.00  54.00 -90.00  126
  3  \w    -62.00 -52.00   1.00   10.00    --  -23.00  72.00-120.00   10
  4  \w   -113.00 -20.00   1.00   10.00    --  -23.00 -18.00 150.00   93
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449676000
_diffrn_orient_matrix_UB_12      -0.0661267000
_diffrn_orient_matrix_UB_13      0.0045863000
_diffrn_orient_matrix_UB_21      -0.0362698000
_diffrn_orient_matrix_UB_22      -0.0680030000
_diffrn_orient_matrix_UB_23      0.0192278000
_diffrn_orient_matrix_UB_31      -0.0125075000
_diffrn_orient_matrix_UB_32      -0.0401779000
_diffrn_orient_matrix_UB_33      -0.0401258000
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1744
_diffrn_reflns_av_unetI/netI     0.1629
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7730
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.567
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24492
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       chip
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0984P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1550
_reflns_number_total             2568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00480c2.cif
_cod_data_source_block           2016fmm7662-33dr
_cod_depositor_comments
'Adding full bibliography for 7046064--7046071.cif.'
_cod_database_code               7046068
_shelxl_version_number           2014-1
_reflns_odcompleteness_completeness 91.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.38
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_olex2_exptl_crystal_mounting_method MiTeGen
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.070
_oxdiff_exptl_absorpt_empirical_full_min 0.188