Pyrazolates advance cerium chemistry: a Ce(III)/Ce(IV) redox equilibrium with benzoquinone.
Werner, Daniel; Deacon, Glen B.; Junk, Peter C.; Anwander, Reiner; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00635g

data_7043769
_publ_section_title
;
 Pyrazolates advance cerium chemistry: a Ce(III)/Ce(IV) redox equilibrium
 with benzoquinone.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00635g
_journal_year                    2017
_chemical_formula_moiety         'C40 H56 Ce2 N16, 0.5(C7 H8)'
_chemical_formula_sum            'C43.5 H60 Ce2 N16'
_chemical_formula_weight         1087.31
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                91.7846(17)
_cell_angle_beta                 96.5974(17)
_cell_angle_gamma                114.0986(16)
_cell_formula_units_Z            2
_cell_length_a                   11.6469(15)
_cell_length_b                   11.8705(15)
_cell_length_c                   19.205(2)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.247
_cell_measurement_theta_min      2.248
_cell_volume                     2398.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.071
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
 wR2(int) was 0.0935 before and 0.0571 after correction. The Ratio 
 of minimum to maximum transmission is 0.8289. The \l/2 correction 
 factor is 0.0000.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         12016
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+1.6190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9521
_reflns_number_total             12016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C43.50 H60 Ce2 N16'
_cod_database_code               7043769
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C2S-C1S \\sim C3S-C2S \\sim C4S-C3S \\sim C5S-C4S \\sim C6S-C5S \\sim C6S-C1S
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C7S, C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C2S(0.5) H2S(0.5) C4S(0.5) H4S(0.5) C1S(0.5) C6S(0.5) H6S(0.5)
 C5S(0.5) H5S(0.5) C3S(0.5) H3S(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5)
5.a Riding coordinates:
 C7S(H7SA,H7SB,H7SC)
5.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C38(H38), C18(H18), C13(H13), C23(H23), C33(H33), C3(H3), C8(H8),
 C2S(H2S), C4S(H4S), C6S(H6S), C5S(H5S), C3S(H3S)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C35(H35A,H35B,H35C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C),
 C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C20(H20A,H20B,H20C), C15(H15A,H15B,
 H15C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C40(H40A,H40B,H40C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              84257
_olex2_submission_special_instructions 'No special instructions were received'