Towards understanding of lanthanide-transition metal bonding: investigations of the first Ce-Fe bonded complex.
Burns, Corey P.; Yang, Xin; Sung, Siyoung; Wofford, Joshua D.; Bhuvanesh, Nattamai S.; Hall, Michael B.; Nippe, Michael; Chemical communications (Cambridge, England) 54 (2018) 10893–10896; doi:10.1039/c8cc05243c

data_7122304
_publ_section_title
;
 Towards understanding of lanthanide-transition metal bonding:
 investigations of the first Ce-Fe bonded complex.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10893
_journal_page_last               10896
_journal_paper_doi               10.1039/c8cc05243c
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H23 Ce F3 N O4 S'
_chemical_formula_sum            'C22 H23 Ce F3 N O4 S'
_chemical_formula_weight         594.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-06-29 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8353(4)
_cell_length_b                   9.9906(3)
_cell_length_c                   15.3663(4)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      31.508
_cell_measurement_theta_min      2.432
_cell_volume                     2277.49(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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      110.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56203
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.990
_diffrn_reflns_theta_min         2.432
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.4350
_exptl_absorpt_correction_T_min  0.3475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0736 before and 0.0449 after correction. The Ratio of minimum to maximum transmission is 0.7989. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.425(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+1.3297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0520
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                6186
_reflns_number_total             8251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05243c2.cif
_cod_data_source_block           mncpb060a
_cod_depositor_comments
'Adding full bibliography for 7122303--7122305.cif.'
_cod_database_code               7122304
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.575(17)
 0.425(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 O4-C18 \\sim O4-C18A
 with sigma of 0.02
 C19-C18A \\sim C19-C18
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C19 \\sim C18 \\sim C18A \\sim O4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C18) = Uanis(C18A)
5. Rigid body (RIGU) restrains
 C19, C18, C18A, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H19C)=Sof(H19D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H19A)=Sof(H19B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C19(H19A,H19B), C19(H19C,H19D),
 C20(H20A,H20B), C21(H21A,H21B), C18A(H18C,H18D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              28829
_olex2_submission_special_instructions 'No special instructions were received'