Coordination of trivalent lanthanum and cerium, and tetravalent cerium and actinides (An = Th(IV), U(IV), Np(IV)) by a 4-phosphoryl 1<i>H</i>-pyrazol-5-olate ligand in solution and the solid state.
Zhang, Jianfeng; Wenzel, Marco; Schnaars, Kathleen; Hennersdorf, Felix; Schwedtmann, Kai; März, Juliane; Rossberg, André; Kaden, Peter; Kraus, Florian; Stumpf, Thorsten; Weigand, Jan J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3550–3558; doi:10.1039/d1dt00365h

data_7706613
_publ_section_title
;
 Coordination of trivalent lanthanum and cerium, and tetravalent cerium
 and actinides (An = Th(IV), U(IV), Np(IV)) by a 4-phosphoryl
 1<i>H</i>-pyrazol-5-olate ligand in solution and the solid state.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3550
_journal_page_last               3558
_journal_paper_doi               10.1039/d1dt00365h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C68 H96 N8 Np O16 P4, 3(C2 H3 N), 2(H3 O1.5)'
_chemical_formula_sum            'C74 H111 N11 Np O19 P4'
_chemical_formula_weight         1819.61
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6551(7)
_cell_length_b                   17.6551(7)
_cell_length_c                   13.7559(6)
_cell_measurement_reflns_used    7710
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4569
_cell_measurement_theta_min      2.2210
_cell_volume                     4287.7(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            99347
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0661 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9449. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             1874
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.278
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0152
_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^)+(0.0189P)^2^+2.1268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             4740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           6_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_cell_volume        4287.7(4)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7706613
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O6
 At 1.5 times of:
  All C(H,H,H) groups, {H6A,H6B} of O6, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O5-H5B = O5-H5A
 0.87 with sigma of 0.001
 C18-H18C_$1 = C18-H18A_$1 = C18-H18B_$1
 0.96 with sigma of 0.001
 H18B-H18A \\sim H18A-H18C \\sim H18B-H18C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N4 \\sim C20 \\sim C21 \\sim N5 \\sim C23 \\sim C22: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{N4, C21, C20} sigma for 1-2: 0.02, 1-3: 0.02
as
{N5, C23, C22}
5. Others
 Fixed Sof: N5(0.25) C23(0.25) C22(0.25) H22A(0.25) H22B(0.25) H22C(0.25)
 H18A(0.25) H18B(0.25) H18C(0.25) N4(0.25) C21(0.25) C20(0.25) H20A(0.25)
 H20B(0.25) H20C(0.25) O5(0.5) O6(0.25) H6A(0.25) H6B(0.25) H5A(0.5) H5B(0.5)
6.a Free rotating group:
 O6(H6A,H6B)
6.b Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              86968
_shelx_hkl_checksum              72223
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'