#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:20:41 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229553 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/60/7046066.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7046066
loop_
_publ_author_name
'Curnock, Emily'
'Levason, William'
'Light, Mark E.'
'Luthra, Sajinder K.'
'McRobbie, Graeme'
'Monzittu, Francesco M.'
'Reid, Gillian'
'Williams, R. Nathan'
_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         'C30 H26 Cl6 La2 N6 O2'
_chemical_formula_sum            'C30 H26 Cl6 La2 N6 O2'
_chemical_formula_weight         993.09
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-04
_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                94.048(3)
_cell_angle_beta                 109.768(3)
_cell_angle_gamma                113.865(4)
_cell_formula_units_Z            1
_cell_length_a                   9.7676(4)
_cell_length_b                   9.9809(4)
_cell_length_c                   10.3396(3)
_cell_measurement_reflns_used    11074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2440
_cell_measurement_theta_min      2.1740
_cell_volume                     841.92(7)
_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(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10844
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.490
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53748
_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_density_diffrn    1.959
_exptl_crystal_description       chunk
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0249
_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/[σ²(Fo²)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3006
_reflns_number_total             3299
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00480c2.cif
_cod_data_source_block           2016rnw7945-05r
_cod_depositor_comments
'Adding full bibliography for 7046064--7046071.cif.'
_cod_original_cell_volume        841.92(6)
_cod_database_code               7046066
_shelxl_version_number           2014-1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 90.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C7(H7), C1(H1), C4(H4), C2(H2), C9(H9), C8(H8), C12(H12),
 C14(H14), C13(H13)
;
_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 3.697
_oxdiff_exptl_absorpt_empirical_full_min 0.200
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
La1 La 0.97564(2) 0.27579(2) 0.37861(2) 0.00972(7) Uani 1 1 d .
Cl1 Cl 0.91659(8) -0.00183(8) 0.22267(8) 0.01363(16) Uani 1 1 d .
Cl3 Cl 1.01034(9) 0.57464(8) 0.36066(8) 0.01666(17) Uani 1 1 d .
Cl2 Cl 1.27268(8) 0.29309(8) 0.56078(8) 0.01763(17) Uani 1 1 d .
O1 O 0.8767(3) 0.0710(3) 0.5099(3) 0.0143(5) Uani 1 1 d .
N1 N 0.6611(3) 0.1918(3) 0.3038(3) 0.0146(6) Uani 1 1 d .
N3 N 1.1282(3) 0.3602(3) 0.2069(3) 0.0117(5) Uani 1 1 d .
N2 N 0.7936(3) 0.2479(3) 0.1085(3) 0.0107(5) Uani 1 1 d .
C10 C 0.8635(3) 0.2833(3) 0.0153(3) 0.0127(6) Uani 1 1 d .
C11 C 1.0408(3) 0.3269(3) 0.0654(3) 0.0122(6) Uani 1 1 d .
C15 C 1.2901(3) 0.4099(3) 0.2534(3) 0.0151(7) Uani 1 1 d .
H15 H 1.3520 0.4352 0.3527 0.018 Uiso 1 1 calc R
C5 C 0.5577(3) 0.1675(3) 0.1691(3) 0.0125(6) Uani 1 1 d .
C3 C 0.3278(4) 0.0824(3) 0.2327(4) 0.0178(7) Uani 1 1 d .
H3 H 0.2136 0.0435 0.2078 0.021 Uiso 1 1 calc R
C7 C 0.5371(4) 0.2005(3) -0.0734(3) 0.0157(7) Uani 1 1 d .
H7 H 0.4235 0.1699 -0.1023 0.019 Uiso 1 1 calc R
C6 C 0.6317(3) 0.2064(3) 0.0639(3) 0.0126(6) Uani 1 1 d .
C1 C 0.5978(4) 0.1631(4) 0.4016(3) 0.0182(7) Uani 1 1 d .
H1 H 0.6701 0.1796 0.4964 0.022 Uiso 1 1 calc R
C4 C 0.3898(3) 0.1110(3) 0.1308(3) 0.0153(7) Uani 1 1 d .
H4 H 0.3188 0.0924 0.0349 0.018 Uiso 1 1 calc R
C2 C 0.4335(4) 0.1109(4) 0.3720(3) 0.0178(7) Uani 1 1 d .
H2 H 0.3943 0.0951 0.4449 0.021 Uiso 1 1 calc R
C9 C 0.7752(4) 0.2816(3) -0.1233(3) 0.0148(7) Uani 1 1 d .
H9 H 0.8277 0.3089 -0.1865 0.018 Uiso 1 1 calc R
C8 C 0.6104(4) 0.2397(3) -0.1674(3) 0.0166(7) Uani 1 1 d .
H8 H 0.5481 0.2379 -0.2613 0.020 Uiso 1 1 calc R
C12 C 1.1142(4) 0.3353(3) -0.0303(3) 0.0155(7) Uani 1 1 d .
H12 H 1.0501 0.3069 -0.1294 0.019 Uiso 1 1 calc R
C14 C 1.3720(4) 0.4265(3) 0.1648(4) 0.0172(7) Uani 1 1 d .
H14 H 1.4875 0.4652 0.2025 0.021 Uiso 1 1 calc R
C13 C 1.2819(4) 0.3855(3) 0.0207(4) 0.0177(7) Uani 1 1 d .
H13 H 1.3340 0.3915 -0.0429 0.021 Uiso 1 1 calc R
H1A H 0.836(4) -0.013(4) 0.467(4) 0.024(11) Uiso 1 1 d .
H1B H 0.942(5) 0.086(4) 0.591(5) 0.029(12) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
Cl1 La1 Cl3 144.65(2) 2_766
Cl1 La1 Cl3 143.98(2) .
Cl3 La1 Cl3 70.77(2) 2_766
Cl2 La1 Cl1 86.82(2) .
Cl2 La1 Cl3 82.93(2) 2_766
Cl2 La1 Cl3 110.27(2) .
O1 La1 Cl1 72.14(6) .
O1 La1 Cl3 72.71(6) 2_766
O1 La1 Cl3 140.69(6) .
O1 La1 Cl2 78.77(6) .
O1 La1 N1 73.83(7) .
O1 La1 N3 145.03(8) .
O1 La1 N2 121.03(7) .
N1 La1 Cl1 92.84(6) .
N1 La1 Cl3 80.87(6) 2_766
N1 La1 Cl3 86.46(6) .
N1 La1 Cl2 151.27(5) .
N1 La1 N3 123.53(7) .
N1 La1 N2 61.59(7) .
N3 La1 Cl1 76.58(6) .
N3 La1 Cl3 135.32(5) 2_766
N3 La1 Cl3 74.01(6) .
N3 La1 Cl2 84.35(6) .
N3 La1 N2 62.21(7) .
N2 La1 Cl1 73.58(6) .
N2 La1 Cl3 74.54(5) .
N2 La1 Cl3 129.74(6) 2_766
N2 La1 Cl2 144.06(6) .
La1 Cl3 La1 109.24(2) 2_766
La1 O1 H1A 116(3) .
La1 O1 H1B 115(3) .
H1A O1 H1B 113(4) .
C5 N1 La1 122.86(19) .
C1 N1 La1 119.1(2) .
C1 N1 C5 117.9(3) .
C11 N3 La1 120.09(17) .
C15 N3 La1 120.76(19) .
C15 N3 C11 118.0(3) .
C10 N2 La1 120.40(19) .
C10 N2 C6 118.3(3) .
C6 N2 La1 121.20(19) .
N2 C10 C11 117.7(3) .
N2 C10 C9 122.1(3) .
C9 C10 C11 120.2(3) .
N3 C11 C10 117.7(3) .
N3 C11 C12 121.5(3) .
C12 C11 C10 120.8(3) .
N3 C15 H15 118.2 .
N3 C15 C14 123.6(3) .
C14 C15 H15 118.2 .
N1 C5 C6 116.9(2) .
N1 C5 C4 121.5(3) .
C4 C5 C6 121.6(3) .
C4 C3 H3 120.3 .
C4 C3 C2 119.4(3) .
C2 C3 H3 120.3 .
C6 C7 H7 120.4 .
C8 C7 H7 120.4 .
C8 C7 C6 119.1(3) .
N2 C6 C5 117.1(3) .
N2 C6 C7 122.2(3) .
C7 C6 C5 120.7(3) .
N1 C1 H1 118.1 .
N1 C1 C2 123.7(3) .
C2 C1 H1 118.1 .
C5 C4 H4 120.2 .
C3 C4 C5 119.5(3) .
C3 C4 H4 120.2 .
C3 C2 H2 121.1 .
C1 C2 C3 117.9(3) .
C1 C2 H2 121.1 .
C10 C9 H9 120.5 .
C8 C9 C10 119.0(3) .
C8 C9 H9 120.5 .
C7 C8 H8 120.4 .
C9 C8 C7 119.3(3) .
C9 C8 H8 120.4 .
C11 C12 H12 120.4 .
C13 C12 C11 119.2(3) .
C13 C12 H12 120.4 .
C15 C14 H14 120.8 .
C13 C14 C15 118.4(3) .
C13 C14 H14 120.8 .
C12 C13 H13 120.4 .
C14 C13 C12 119.2(3) .
C14 C13 H13 120.4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 Cl1 2.8385(8) .
La1 Cl3 2.9209(8) 2_766
La1 Cl3 2.8894(7) .
La1 Cl2 2.8014(8) .
La1 O1 2.576(2) .
La1 N1 2.638(2) .
La1 N3 2.659(2) .
La1 N2 2.677(2) .
Cl3 La1 2.9210(8) 2_766
O1 H1A 0.78(4) .
O1 H1B 0.83(4) .
N1 C5 1.349(4) .
N1 C1 1.344(4) .
N3 C11 1.355(4) .
N3 C15 1.340(4) .
N2 C10 1.349(4) .
N2 C6 1.355(4) .
C10 C11 1.486(4) .
C10 C9 1.395(4) .
C11 C12 1.394(4) .
C15 H15 0.9500 .
C15 C14 1.385(4) .
C5 C6 1.490(4) .
C5 C4 1.395(4) .
C3 H3 0.9500 .
C3 C4 1.376(4) .
C3 C2 1.386(5) .
C7 H7 0.9500 .
C7 C6 1.389(4) .
C7 C8 1.381(4) .
C1 H1 0.9500 .
C1 C2 1.382(4) .
C4 H4 0.9500 .
C2 H2 0.9500 .
C9 H9 0.9500 .
C9 C8 1.380(4) .
C8 H8 0.9500 .
C12 H12 0.9500 .
C12 C13 1.389(4) .
C14 H14 0.9500 .
C14 C13 1.377(5) .
C13 H13 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
La1 N1 C5 C6 -6.5(4)
La1 N1 C5 C4 174.5(2)
La1 N1 C1 C2 -176.5(2)
La1 N3 C11 C10 17.0(3)
La1 N3 C11 C12 -164.0(2)
La1 N3 C15 C14 166.5(2)
La1 N2 C10 C11 4.4(3)
La1 N2 C10 C9 -174.9(2)
La1 N2 C6 C5 -3.8(3)
La1 N2 C6 C7 175.8(2)
N1 C5 C6 N2 6.6(4)
N1 C5 C6 C7 -173.0(3)
N1 C5 C4 C3 1.5(5)
N1 C1 C2 C3 2.0(5)
N3 C11 C12 C13 -3.0(4)
N3 C15 C14 C13 -2.0(5)
N2 C10 C11 N3 -14.1(4)
N2 C10 C11 C12 166.9(3)
N2 C10 C9 C8 -1.2(5)
C10 N2 C6 C5 179.8(3)
C10 N2 C6 C7 -0.5(4)
C10 C11 C12 C13 176.0(3)
C10 C9 C8 C7 -0.1(5)
C11 N3 C15 C14 -1.2(4)
C11 C10 C9 C8 179.6(3)
C11 C12 C13 C14 -0.3(4)
C15 N3 C11 C10 -175.3(3)
C15 N3 C11 C12 3.7(4)
C15 C14 C13 C12 2.7(4)
C5 N1 C1 C2 -0.3(5)
C6 N2 C10 C11 -179.3(3)
C6 N2 C10 C9 1.5(4)
C6 C5 C4 C3 -177.4(3)
C6 C7 C8 C9 1.0(5)
C1 N1 C5 C6 177.5(3)
C1 N1 C5 C4 -1.5(4)
C4 C5 C6 N2 -174.4(3)
C4 C5 C6 C7 5.9(4)
C4 C3 C2 C1 -1.9(5)
C2 C3 C4 C5 0.3(5)
C9 C10 C11 N3 165.2(3)
C9 C10 C11 C12 -13.8(4)
C8 C7 C6 N2 -0.7(5)
C8 C7 C6 C5 178.9(3)
