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_7706612
_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 H97 La N8 O16 P4, 0.75(C8 H12 N4), 3(H2 O)'
_chemical_formula_sum            'C74 H112 La N11 O19 P4'
_chemical_formula_weight         1722.53
_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                   17.80376(5)
_cell_length_b                   17.80376(5)
_cell_length_c                   13.75097(7)
_cell_measurement_reflns_used    31995
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      76.5650
_cell_measurement_theta_min      3.5020
_cell_volume                     4358.70(3)
_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      100.0(3)
_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 0.998
_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  32.00   0.50    0.50    --  -38.50  57.00  60.00  186
  2  \w    -60.00 -33.00   0.50    0.50    --  -38.50  77.00-180.00   54
  3  \w    -15.00  26.00   0.50    0.50    --  -38.50  77.00-180.00   82
  4  \w     20.00  83.00   0.50    0.50    --   42.75  38.00-180.00  126
  5  \w     41.00  75.00   0.50    2.00    --  111.00 -45.00 -90.00   68
  6  \w     94.00 123.00   0.50    2.00    --  111.00 -45.00 -90.00   58
  7  \w    109.00 136.00   0.50    2.00    --  111.00 -77.00   0.00   54
  8  \w     96.00 121.00   0.50    2.00    --  111.00-125.00  30.00   50
  9  \w     78.00 105.00   0.50    2.00    --  111.00-125.00   0.00   54
 10  \w     64.00 101.00   0.50    2.00    --  111.00 -94.00  30.00   74
 11  \w     56.00  83.00   0.50    2.00    --  111.00-125.00  30.00   54
 12  \w     52.00  79.00   0.50    2.00    --  111.00-125.00  60.00   54
 13  \w     72.00 121.00   0.50    2.00    --  111.00-125.00 120.00   98
 14  \w     41.00 135.00   0.50    2.00    --  111.00 -45.00  30.00  188
 15  \w     61.00  88.00   0.50    2.00    --  111.00 -94.00-120.00   54
 16  \w     73.00 120.00   0.50    2.00    --  111.00-125.00-120.00   94
 17  \w     62.00  89.00   0.50    2.00    --  111.00 -61.00-150.00   54
 18  \w     53.00 115.00   0.50    2.00    --  111.00-125.00-180.00  124
 19  \w     53.00 121.00   0.50    2.00    --  111.00-125.00 -60.00  136
 20  \w     38.00  97.00   0.50    0.50    --   42.75-125.00-180.00  118
 21  \w     36.00  77.00   0.50    0.50    --   42.75-125.00 -90.00   82
 22  \w     37.00  84.00   0.50    2.00    --  111.00 -94.00-180.00   94
 23  \w     35.00 153.00   0.50    2.00    --  111.00 -15.00-120.00  236
 24  \w     39.00 107.00   0.50    2.00    --  111.00-125.00 -30.00  136
 25  \w     39.00  92.00   0.50    2.00    --  111.00 -94.00   0.00  106
 26  \w     31.00 154.00   0.50    2.00    --  111.00 -15.00   0.00  246
 27  \w     40.00 135.00   0.50    2.00    --  111.00 -45.00 150.00  190
 28  \w     30.00 109.00   0.50    2.00    --  111.00 -94.00  60.00  158
 29  \w     31.00 156.00   0.50    2.00    --  111.00 -15.00 120.00  250
 30  \w   -109.00 -12.00   0.50    0.50    --  -38.50 -57.00 -90.00  194
;
_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      -0.0047782000
_diffrn_orient_matrix_UB_12      0.0270919000
_diffrn_orient_matrix_UB_13      0.1062664000
_diffrn_orient_matrix_UB_21      -0.0732933000
_diffrn_orient_matrix_UB_22      0.0423285000
_diffrn_orient_matrix_UB_23      -0.0235624000
_diffrn_orient_matrix_UB_31      -0.0459099000
_diffrn_orient_matrix_UB_32      -0.0702628000
_diffrn_orient_matrix_UB_33      0.0268405000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.693
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.058
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.353
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0196
_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^)+(0.0326P)^2^+1.2051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4556
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7706612
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C156 H192 La2 N22 O40 P8 '
_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 N(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H5AA-N2
 2.1 with sigma of 0.02
 O5A-H5AB
 0.85 with sigma of 0.01
 H14A-O5B_$1
 -2 with sigma of 0.02
 H2-O5A
 1.96 with sigma of 0.01
 C18-H18C = C18-H18B = C18-H18A = N2-H2
 0.96 with sigma of 0.001
 H18C-H18B \\sim H18B-H18A \\sim H18C-H18A
 with sigma of 0.01
3. Same fragment restrains
{C23, C22, N5} sigma for 1-2: 0.02, 1-3: 0.02
{C21, C20, N4} sigma for 1-2: 0.02, 1-3: 0.02
as
{C18, C19, N3}
4. Others
 Fixed Sof: H18A(0.25) H18B(0.25) H18C(0.25) H2(0.25) N4(0.25) C20(0.25)
 C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) C22(0.25) C23(0.25) H23A(0.25)
 H23B(0.25) H23C(0.25) N5(0.25) O5B(0.25) H5BA(0.25) H5BB(0.25) O5A(0.5)
 H5AA(0.5) H5AB(0.5)
5.a Free rotating group:
 O5B(H5BA,H5BB), O5A(H5AA,H5AB)
5.b Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10)
5.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), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              46010
_shelx_hkl_checksum              47798
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.772