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_7046071
_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         'C15 H13 Cl3 Lu N3 O'
_chemical_formula_sum            'C15 H13 Cl3 Lu N3 O'
_chemical_formula_weight         532.60
_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   mixed
_audit_creation_date             2017-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.953(7)
_cell_angle_beta                 82.993(6)
_cell_angle_gamma                72.341(6)
_cell_formula_units_Z            2
_cell_length_a                   7.5588(5)
_cell_length_b                   10.0003(7)
_cell_length_c                   12.0814(9)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1020
_cell_measurement_theta_min      2.2800
_cell_volume                     817.31(11)
_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      100.15
_diffrn_detector                 'CCD plate'
_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  67.00   1.00   10.00    --  -23.00   0.00 -60.00  180
  2  \w    -87.00  16.00   1.00   10.00    --  -23.00 -72.00 120.00  103
  3  \w    -69.00  16.00   1.00   10.00    --  -23.00 -72.00-120.00   85
  4  \w    -34.00   4.00   1.00   10.00    --  -23.00  72.00   0.00   38
  5  \w    -57.00 -13.00   1.00   10.00    --  -23.00 -72.00  60.00   44
  6  \w    -39.00  67.00   1.00   10.00    --  -23.00  72.00 -60.00  106
  7  \w    -73.00  16.00   1.00   10.00    --  -23.00 -72.00-180.00   89
  8  \w    -75.00  16.00   1.00   10.00    --  -23.00 -72.00   0.00   91
  9  \w    -69.00  26.00   1.00   10.00    --  -23.00   0.00 -30.00   95
 10  \w    -31.00  -7.00   1.00   10.00    --  -23.00  72.00 120.00   24
 11  \w    -39.00 -28.00   1.00   10.00    --  -23.00  72.00 -90.00   11
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0463927000
_diffrn_orient_matrix_UB_12      -0.0603265000
_diffrn_orient_matrix_UB_13      0.0478514000
_diffrn_orient_matrix_UB_21      0.0819128000
_diffrn_orient_matrix_UB_22      0.0234509000
_diffrn_orient_matrix_UB_23      -0.0154714000
_diffrn_orient_matrix_UB_31      -0.0289745000
_diffrn_orient_matrix_UB_32      0.0446954000
_diffrn_orient_matrix_UB_33      0.0371280000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            12609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.259
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24120
_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    2.164
_exptl_crystal_description       chunk
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.019
_refine_diff_density_max         2.977
_refine_diff_density_min         -2.946
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3214
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0603P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2859
_reflns_number_total             3214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00480c2.cif
_cod_data_source_block           2016rnw7945-09ar
_cod_depositor_comments
'Adding full bibliography for 7046064--7046071.cif.'
_cod_original_cell_volume        817.32(10)
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               7046071
_shelxl_version_number           2014-1
_cell_oxdiff_angle_alpha         69.953(7)
_cell_oxdiff_angle_beta          82.993(6)
_cell_oxdiff_angle_gamma         72.341(6)
_cell_oxdiff_length_a            7.5588(5)
_cell_oxdiff_length_b            10.0003(7)
_cell_oxdiff_length_c            12.0814(9)
_cell_oxdiff_measurement_reflns_used 9792
_cell_oxdiff_volume              817.32(10)
_reflns_odcompleteness_completeness 92.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.31
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15)
2.c Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C6,C7,C8,C9,C10), N3(C11,C12,C13,C14,C15)
;
_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 4.061
_oxdiff_exptl_absorpt_empirical_full_min 0.115