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_7046070
_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         '2(C9 H21 I2 N3 O0.5 Y), C2 H3 N'
_chemical_formula_sum            'C20 H45 I4 N7 O Y2'
_chemical_formula_weight         1085.05
_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     heavy
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.160(3)
_cell_angle_beta                 90.941(3)
_cell_angle_gamma                108.966(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6352(3)
_cell_length_b                   8.6395(3)
_cell_length_c                   23.7313(8)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0750
_cell_measurement_theta_min      2.4580
_cell_volume                     1674.04(10)
_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_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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   1.00   1.00   10.00    --  -23.00 -18.00   0.00  114
  2  \w    -62.00  53.00   1.00   10.00    --  -23.00  72.00 120.00  115
  3  \w    -88.00  15.00   1.00   10.00    --  -23.00 -72.00 -60.00  103
  4  \w    -39.00 -27.00   1.00    5.00    --  -23.00 -72.00-120.00   12
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0183563000
_diffrn_orient_matrix_UB_12      -0.0308259000
_diffrn_orient_matrix_UB_13      0.0276391000
_diffrn_orient_matrix_UB_21      0.0740451000
_diffrn_orient_matrix_UB_22      -0.0188341000
_diffrn_orient_matrix_UB_23      0.0011280000
_diffrn_orient_matrix_UB_31      0.0415589000
_diffrn_orient_matrix_UB_32      0.0789425000
_diffrn_orient_matrix_UB_33      0.0113412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11161
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78914
_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            yellow
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0370P)^2^+5.4138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5686
_reflns_number_total             6471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00480c2.cif
_cod_data_source_block           2016fmm7662-37ar
_cod_depositor_comments
'Adding full bibliography for 7046064--7046071.cif.'
_cod_original_cell_volume        1674.05(10)
_cod_database_code               7046070
_shelxl_version_number           2014-1
_reflns_odcompleteness_completeness 85.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.31
_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:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B), C12(H12A,H12B), C5(H5A,H5B), C4(H4A,
 H4B), C6(H6A,H6B), C10(H10A,H10B), C11(H11A,H11B), C15(H15A,H15B), C13(H13A,
 H13B), C14(H14A,H14B)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C),
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              64513
_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 3.177
_oxdiff_exptl_absorpt_empirical_full_min 0.407