Synthesis and structural, redox and photophysical properties of tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
McPherson, James N.; Abad Galan, Laura; Iranmanesh, Hasti; Massi, Massimiliano; Colbran, Stephen B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9365–9375; doi:10.1039/c9dt01262a

data_7700168
_publ_section_title
;
 Synthesis and structural, redox and photophysical properties of
 tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9365
_journal_page_last               9375
_journal_paper_doi               10.1039/c9dt01262a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H42 La N9, 1.5(C6 H6)'
_chemical_formula_sum            'C57 H51 La N9'
_chemical_formula_weight         1000.98
_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     dual
_audit_creation_date             2017-11-15
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                80.97(3)
_cell_angle_beta                 83.88(3)
_cell_angle_gamma                70.72(3)
_cell_formula_units_Z            2
_cell_length_a                   12.928(3)
_cell_length_b                   13.980(3)
_cell_length_c                   14.100(3)
_cell_measurement_reflns_used    10228
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.876
_cell_measurement_theta_min      1.556
_cell_volume                     2371.5(10)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39500
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         1.556
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             1026
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.505
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0198(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         10228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+2.6418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9722
_reflns_number_total             10228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01262a2.cif
_cod_data_source_block           p1bar_a
_cod_depositor_comments
'Adding full bibliography for 7700168--7700170.cif.'
_cod_original_cell_volume        2371.5(9)
_cod_database_code               7700168
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1C(H1C), C2A(H2A), C2B(H2B), C2C(H2C), C3A(H3A),
 C3B(H3B), C3C(H3C), C4A(H4A), C4B(H4B), C4C(H4C), C13A(H13A), C13B(H13B),
 C13C(H13C), C14A(H14A), C14B(H14B), C14C(H14C), C15A(H15A), C15B(H15B),
 C15C(H15C), C16A(H16A), C16B(H16B), C16C(H16C), C1(H1), C2(H2), C3(H3), C4(H4),
  C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC), C8C(H8CA,H8CB,H8CC), C9A(H9AA,H9AB,
 H9AC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC)
;
_olex2_submission_special_instructions 'No special instructions were received'