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_7043777
_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         'C66 H114 Ce2 N12, 2(C7 H8)'
_chemical_formula_sum            'C80 H130 Ce2 N12'
_chemical_formula_weight         1540.19
_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     iterative
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                119.1810(10)
_cell_angle_beta                 96.4120(10)
_cell_angle_gamma                95.2750(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4097(10)
_cell_length_b                   13.7574(11)
_cell_length_c                   13.9173(11)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.907
_cell_measurement_theta_min      2.380
_cell_volume                     2031.9(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.675
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8238.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9326
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0309
_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/[\s^2^(Fo^2^)+(0.0324P)^2^+1.8500P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8184
_reflns_number_total             9326
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {d2028176-4172-4afc-97e4-766dc85c74a0}
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           3
_cod_database_code               7043777
_shelxl_version_number           2013-2
_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. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3. Others
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C48)=Sof(H48)=Sof(C38)=Sof(H38)=
 Sof(C40)=Sof(H40)=Sof(C44)=Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=1-FVAR(1)
 Sof(C49)=Sof(H49)=Sof(C47)=Sof(H47)=Sof(C41)=Sof(H41)=Sof(C6AA)=Sof(C39)=
 Sof(H39)=Sof(C37)=Sof(H37)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C49(H49), C47(H47), C8(H8), C13(H13), C3(H3), C41(H41), C39(H39), C37(H37),
 C48(H48), C38(H38), C40(H40), C46(H46), C45(H45)
4.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C21(H21A,
 H21B,H21C), C18(H18A,H18B,H18C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C19(H19A,H19B,H19C), C36(H36A,H36B,
 H36C), C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C24(H24A,H24B,H24C), C22(H22A,
 H22B,H22C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C),
 C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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