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_7043770
_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         'C62 H79 Ce3 N20 O4'
_chemical_formula_sum            'C62 H79 Ce3 N20 O4'
_chemical_formula_weight         1588.81
_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
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                96.1130(10)
_cell_angle_beta                 94.7260(10)
_cell_angle_gamma                106.0150(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1911(10)
_cell_length_b                   15.5304(14)
_cell_length_c                   20.5161(18)
_cell_measurement_reflns_used    9610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.788
_cell_measurement_theta_min      2.554
_cell_volume                     3384.5(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      99.9
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21728
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         4.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0566 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.9345.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         11598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.4070P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9587
_reflns_number_total             11598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           5b
_cod_database_code               7043770
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C40(H40), C8(H8), N19(H19), C23(H23), C26(H26), C19(H19A), C3(H3), C30(H30),
 C50(H50), C14(H14), C25(H25), C45(H45), C7(H7), C9(H9), C24(H24), C55(H55),
 C60(H60), C10(H10), C35(H35)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C38(H38A,H38B,H38C), C57(H57A,H57B,H57C), C48(H48A,H48B,
 H48C), C28(H28A,H28B,H28C), C21(H21A,H21B,H21C), C52(H52A,H52B,H52C), C62(H62A,
 H62B,H62C), C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C1(H1A,H1B,H1C), C42(H42A,
 H42B,H42C), C58(H58A,H58B,H58C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C43(H43A,H43B,H43C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              38063
_olex2_submission_special_instructions 'No special instructions were received'