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_7043768
_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_absolute_configuration ad
_chemical_formula_moiety         'C65 H87 N18 O6 Pr3, 2(C4 H8 O)'
_chemical_formula_sum            'C73 H103 N18 O8 Pr3'
_chemical_formula_weight         1783.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1890(3)
_cell_length_b                   20.1148(4)
_cell_length_c                   23.3716(4)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.38
_cell_volume                     7610.7(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            111020
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0643 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.9292.
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    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         18228
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+10.0056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                16734
_reflns_number_total             18228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           5aPr
_cod_database_code               7043768
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C65(H65A,H65B), C62(H62A,H62B), C60(H60A,H60B), C64(H64A,
 H64B), C58(H58A,H58B), C71(H71A,H71B), C59(H59A,H59B), C73(H73A,H73B),
 C63(H63A,H63B), C70(H70A,H70B), C69(H69A,H69B), C68(H68A,H68B), C72(H72A,H72B),
  C66(H66A,H66B), C67(H67A,H67B)
3.b Me refined with riding coordinates:
 C53(H53A,H53B,H53C)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C7(H7), C25(H25), C9(H9), C35(H35), C26(H26), C23(H23),
 C45(H45), C40(H40), C24(H24), C8(H8), C30(H30), C55(H55), C19(H19), C14(H14),
 C50(H50)
3.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C16(H16A,H16B,
 H16C), C57(H57A,H57B,H57C), C38(H38A,H38B,H38C), C43(H43A,H43B,H43C), C5(H5A,
 H5B,H5C), C21(H21A,H21B,H21C), C47(H47A,H47B,H47C), C42(H42A,H42B,H42C),
 C37(H37A,H37B,H37C), C52(H52A,H52B,H52C), C12(H12A,H12B,H12C), C28(H28A,H28B,
 H28C), C48(H48A,H48B,H48C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'