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_7706611
_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 Th, 0.75(C8 H12 N4), 3(H2 O)'
_chemical_formula_sum            'C74 H111 N11 O19 P4 Th'
_chemical_formula_weight         1814.65
_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             2021-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-06 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                   17.74494(4)
_cell_length_b                   17.74494(4)
_cell_length_c                   13.70378(6)
_cell_measurement_reflns_used    50622
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      76.4530
_cell_measurement_theta_min      3.2280
_cell_volume                     4315.09(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      100.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -61.00  34.00   1.00    3.00    --  -38.50  38.00 -30.00   95
  2  \w    -65.00  32.00   1.00    3.00    --  -38.50  57.00-180.00   97
  3  \w     26.00  56.00   1.00    3.00    --   42.62-125.00-120.00   30
  4  \w     57.00  97.00   1.00    3.00    --   42.62-125.00 -30.00   40
  5  \w     48.00  75.00   1.00   12.00    --  111.00-125.00   0.00   27
  6  \w     81.00 121.00   1.00   12.00    --  111.00-125.00   0.00   40
  7  \w     95.00 121.00   1.00   12.00    --  111.00-125.00 -60.00   26
  8  \w    113.00 142.00   1.00   12.00    --  111.00 -77.00 -60.00   29
  9  \w     95.00 123.00   1.00   12.00    --  111.00 -64.00-128.94   28
 10  \w    103.00 130.00   1.00   12.00    --  111.00 -45.00-150.00   27
 11  \w     87.00 132.00   1.00   12.00    --  111.00 -47.00-127.23   45
 12  \w     88.00 115.00   1.00   12.00    --  111.00  15.00 -60.00   27
 13  \w    134.00 178.00   1.00   12.00    --  111.00  15.00 -30.00   44
 14  \w    147.00 174.00   1.00   12.00    --  111.00  15.00 -60.00   27
 15  \w    144.00 171.00   1.00   12.00    --  111.00  61.00-120.00   27
 16  \w    147.00 177.00   1.00   12.00    --  111.00  77.00-120.00   30
 17  \w    139.00 166.00   1.00   12.00    --  111.00 125.00 -60.00   27
 18  \w    133.00 169.00   1.00   12.00    --  111.00 125.00 -30.00   36
 19  \w    147.00 174.00   1.00   12.00    --  111.00 125.00  60.00   27
 20  \w    138.00 165.00   1.00   12.00    --  111.00 125.00 150.00   27
 21  \w     94.00 134.00   1.00   12.00    --  111.00  45.00 120.00   40
 22  \w    104.00 141.00   1.00   12.00    --  111.00  15.00  90.00   37
 23  \w    142.00 169.00   1.00   12.00    --  111.00  30.00  30.00   27
 24  \w    111.00 174.00   1.00   12.00    --  111.00  30.00   0.00   63
 25  \w    110.00 137.00   1.00   12.00    --  111.00  61.00-120.00   27
 26  \w    135.00 177.00   1.00   12.00    --  111.00  77.00-180.00   42
 27  \w    121.00 149.00   1.00   12.00    --  111.00 125.00-150.00   28
 28  \w     95.00 121.00   1.00   12.00    --  111.00 125.00 -60.00   26
 29  \w     91.00 118.00   1.00   12.00    --  111.00  77.00-120.00   27
 30  \w     98.00 132.00   1.00   12.00    --  111.00  45.00 -90.00   34
 31  \w     90.00 137.00   1.00   12.00    --  111.00  45.00-180.00   47
 32  \w     82.00 107.00   1.00   12.00    --  111.00  77.00-150.00   25
 33  \w     67.00  92.00   1.00   12.00    --  111.00  15.00-150.00   25
 34  \w     68.00 176.00   1.00   12.00    --  111.00  15.00 -90.00  108
 35  \w     87.00 114.00   1.00   12.00    --  111.00 -45.00   0.00   27
 36  \w     75.00 107.00   1.00   12.00    --  111.00 -94.00  30.00   32
 37  \w     85.00 121.00   1.00   12.00    --  111.00-125.00  60.00   36
 38  \w     96.00 121.00   1.00   12.00    --  111.00-125.00 120.00   25
 39  \w     96.00 141.00   1.00   12.00    --  111.00 -77.00 150.00   45
 40  \w    120.00 153.00   1.00   12.00    --  111.00 -15.00 150.00   33
 41  \w     91.00 118.00   1.00   12.00    --  111.00 -61.00 120.00   27
 42  \w     81.00 108.00   1.00   12.00    --  111.00 -77.00 120.00   27
 43  \w     89.00 119.00   1.00   12.00    --  111.00-125.00 150.00   30
 44  \w     78.00 104.00   1.00   12.00    --  111.00 -94.00 120.00   26
 45  \w     78.00 109.00   1.00   12.00    --  111.00 -94.00  60.00   31
 46  \w     68.00 101.00   1.00   12.00    --  111.00 -94.00 150.00   33
 47  \w     64.00  91.00   1.00   12.00    --  111.00 -61.00  90.00   27
 48  \w     58.00  85.00   1.00   12.00    --  111.00 -77.00 150.00   27
 49  \w     49.00  74.00   1.00   12.00    --  111.00-125.00 120.00   25
 50  \w     39.00  64.00   1.00   12.00    --  111.00 -77.00 120.00   25
 51  \w     37.00  64.00   1.00   12.00    --  111.00 -94.00 150.00   27
 52  \w     40.00 114.00   1.00   12.00    --  111.00 -51.00 174.60   74
 53  \w     72.00  99.00   1.00   12.00    --  111.00  15.00  90.00   27
 54  \w     86.00 112.00   1.00   12.00    --  111.00  55.00  26.00   26
 55  \w     50.00  77.00   1.00   12.00    --  111.00 -30.00 -30.00   27
 56  \w     65.00 114.00   1.00   12.00    --  111.00 -61.00 -30.00   49
 57  \w     75.00 103.00   1.00   12.00    --  111.00 -94.00-120.00   28
 58  \w     94.00 121.00   1.00   12.00    --  111.00-125.00-180.00   27
 59  \w     68.00 121.00   1.00   12.00    --  111.00-125.00-120.00   53
 60  \w     62.00 101.00   1.00   12.00    --  111.00 -94.00   0.00   39
 61  \w     67.00  94.00   1.00   12.00    --  111.00 -61.00   0.00   27
 62  \w     54.00 139.00   1.00   12.00    --  111.00 -61.00  30.00   85
 63  \w     62.00 117.00   1.00   12.00    --  111.00-125.00  30.00   55
 64  \w     48.00  73.00   1.00   12.00    --  111.00-125.00 -60.00   25
 65  \w     45.00 108.00   1.00   12.00    --  111.00-125.00 -30.00   63
 66  \w     52.00 109.00   1.00   12.00    --  111.00-125.00 -90.00   57
 67  \w     58.00  85.00   1.00   12.00    --  111.00-125.00-180.00   27
 68  \w     50.00  84.00   1.00   12.00    --  111.00 -47.00-127.23   34
 69  \w     40.00  66.00   1.00   12.00    --  111.00 -77.00 -60.00   26
 70  \w     40.00  67.00   1.00   12.00    --  111.00 -77.00 -30.00   27
 71  \w     42.00  67.00   1.00   12.00    --  111.00 -45.00   0.00   25
 72  \w     39.00  96.00   1.00   12.00    --  111.00 -30.00   0.00   57
 73  \w     42.00  93.00   1.00   12.00    --  111.00 -22.00  96.01   51
 74  \w     31.00  56.00   1.00   12.00    --  111.00 -94.00   0.00   25
 75  \w     32.00  64.00   1.00   12.00    --  111.00 -94.00  30.00   32
 76  \w     30.00  81.00   1.00   12.00    --  111.00 -94.00 -30.00   51
 77  \w   -109.00 -14.00   1.00    3.00    --  -38.50 -57.00  30.00   95
;
_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      0.0679247000
_diffrn_orient_matrix_UB_12      -0.0403412000
_diffrn_orient_matrix_UB_13      -0.0467081000
_diffrn_orient_matrix_UB_21      -0.0159085000
_diffrn_orient_matrix_UB_22      0.0404216000
_diffrn_orient_matrix_UB_23      -0.0973206000
_diffrn_orient_matrix_UB_31      0.0517169000
_diffrn_orient_matrix_UB_32      0.0653762000
_diffrn_orient_matrix_UB_33      0.0313190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            82081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.813
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0230P)^2^+3.2413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4488
_reflns_number_total             4563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           7_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_cell_volume        4315.09(3)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7706611
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O P Th'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 H5BA-N2
 2 with sigma of 0.02
 C18-H18C_$1 = C18-H18B_$1 = C18-H18A_$1
 0.96 with sigma of 0.001
 H18C-H18B \\sim H18B-H18A \\sim H18C-H18A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N4 \\sim C21 \\sim C20 \\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
{N5, C23, C22} sigma for 1-2: 0.02, 1-3: 0.02
as
{N3, C19, C18}
5. Others
 Fixed Sof: H18A(0.25) H18B(0.25) H18C(0.25) O5B(0.5) H5BA(0.5) H5BB(0.5)
 O5A(0.25) H5AA(0.25) H5AB(0.25) N5(0.25) C23(0.25) C22(0.25) H22A(0.25)
 H22B(0.25) H22C(0.25) N4(0.25) C21(0.25) C20(0.25) H20A(0.25) H20B(0.25)
 H20C(0.25)
6.a Free rotating group:
 O5B(H5BA,H5BB), O5A(H5AA,H5AB)
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 with riding coordinates:
 C22(H22A,H22B,H22C)
6.e Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              35063
_shelx_hkl_checksum              64407
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.825