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_7706610
_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 O16 P4 U, 3(C2 H3 N), 2(H3 O1.5)'
_chemical_formula_sum            'C74 H111 N11 O19 P4 U'
_chemical_formula_weight         1820.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 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                   17.68430(10)
_cell_length_b                   17.68430(10)
_cell_length_c                   13.7690(2)
_cell_measurement_reflns_used    16571
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.0070
_cell_measurement_theta_min      3.1980
_cell_volume                     4306.04(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -21.00  68.00   0.50    2.00    --   42.50 -81.00 140.00  178
  2  \w    101.00 129.00   0.50    8.00    --  111.00 -81.00 140.00   56
  3  \w    116.00 177.00   0.50    8.00    --  111.00  81.00 -97.00  122
  4  \w     44.00  69.00   0.50    8.00    --  111.00 -81.00 140.00   50
  5  \w    -70.00  35.00   0.50    2.00    --  -38.50  81.00 -97.00  210
  6  \w    -81.00 -27.00   0.50    2.00    --  -38.50 -57.00  90.00  108
  7  \w    -47.00  -8.00   0.50    2.00    --  -38.50 125.00 150.00   78
  8  \w    -70.00  35.00   0.50    2.00    --  -38.50  77.00  30.00  210
  9  \w    -29.00  24.00   0.50    2.00    --   42.50 -38.00 -30.00  106
 10  \w     38.00  63.00   0.50    2.00    --   42.50 -38.00 -30.00   50
 11  \w    -20.00   6.00   0.50    2.00    --   42.50 -77.00  60.00   52
 12  \w     22.00  49.00   0.50    2.00    --   42.50 -77.00  60.00   54
 13  \w     49.00  76.00   0.50    8.00    --  111.00 -94.00-150.00   54
 14  \w     30.00 106.00   0.50    8.00    --  111.00 -94.00 120.00  152
 15  \w     80.00 107.00   0.50    8.00    --  111.00 -94.00 -60.00   54
 16  \w    108.00 177.00   0.50    8.00    --  111.00  77.00 -60.00  138
 17  \w     81.00 107.00   0.50    8.00    --  111.00 -94.00-150.00   52
 18  \w     44.00  79.00   0.50    8.00    --  111.00-125.00 -90.00   70
 19  \w     40.00 111.00   0.50    8.00    --  111.00-125.00 120.00  142
 20  \w    104.00 177.00   0.50    8.00    --  111.00  77.00 -30.00  146
 21  \w     97.00 124.00   0.50    8.00    --  111.00  30.00 -60.00   54
 22  \w     39.00  77.00   0.50    8.00    --  111.00 -94.00 -60.00   76
 23  \w    137.00 165.00   0.50    8.00    --  111.00  61.00-180.00   56
 24  \w    145.00 172.00   0.50    8.00    --  111.00  30.00 -60.00   54
 25  \w     79.00 106.00   0.50    8.00    --  111.00 -94.00-180.00   54
 26  \w     30.00  42.50   0.50    8.00    --  111.00 -94.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0424217000
_diffrn_orient_matrix_UB_12      -0.0697743000
_diffrn_orient_matrix_UB_13      0.0388439000
_diffrn_orient_matrix_UB_21      -0.0123285000
_diffrn_orient_matrix_UB_22      -0.0279619000
_diffrn_orient_matrix_UB_23      -0.1048359000
_diffrn_orient_matrix_UB_31      0.0750937000
_diffrn_orient_matrix_UB_32      -0.0439736000
_diffrn_orient_matrix_UB_33      0.0049752000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.916
_diffrn_reflns_theta_min         3.210
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.592
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0587P)^2^+4.5348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4349
_reflns_number_total             4509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_cell_volume        4306.04(8)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7706610
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C74H113N11NUO20P4 '
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.539
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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,H5A,H5B)
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              58304
_shelx_hkl_checksum              1565
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.615