Stoichiometric control: 8- and 10-coordinate Ln(hfac)<sub>3</sub>(bpy) and Ln(hfac)<sub>3</sub>(bpy)<sub>2</sub> complexes of the early lanthanides La-Sm.
Fatila, Elisabeth M.; Maahs, Adam C.; Hetherington, Erin E.; Cooper, Brandon J.; Cooper, Riley E.; Daanen, Nick N.; Jennings, Michael; Skrabalak, Sara E.; Preuss, Kathryn E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16232–16241; doi:10.1039/c8dt03286f

data_7047850
_publ_section_title
;
 Stoichiometric control: 8- and 10-coordinate Ln(hfac)<sub>3</sub>(bpy)
 and Ln(hfac)<sub>3</sub>(bpy)<sub>2</sub> complexes of the early
 lanthanides La-Sm.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16232
_journal_page_last               16241
_journal_paper_doi               10.1039/c8dt03286f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C35 H19 Ce F18 N4 O6'
_chemical_formula_sum            'C35 H19 Ce F18 N4 O6'
_chemical_formula_weight         1073.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.98(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.819(4)
_cell_length_b                   11.828(2)
_cell_length_c                   18.116(4)
_cell_measurement_reflns_used    23613
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     4089.9(18)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20806
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.570
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylene chloride/hexanes'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3617
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+32.7423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2959
_reflns_number_total             3617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03286f2.cif
_cod_data_source_block           k11163
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047848--7047856.cif.
;
_cod_database_code               7047850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.605
_shelx_estimated_absorpt_t_max   0.707
_shelx_res_checksum              39960