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_7706617
_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'
_chemical_formula_sum            'C68 H96 N8 O16 P4 U'
_chemical_formula_weight         1643.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-02 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1117(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.05395(19)
_cell_length_b                   13.02519(5)
_cell_length_c                   36.6159(2)
_cell_measurement_reflns_used    103494
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3640
_cell_measurement_theta_min      2.5990
_cell_volume                     15000.87(14)
_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      100.00(10)
_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 0.992
_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    -54.00  14.00   0.50    4.00    --  -38.50  98.00 -92.00  136
  2  \w     35.00  81.00   0.50    4.00    --   42.50 -98.00 160.00   92
  3  \w     77.00 106.00   0.50   16.00    --  111.00 -98.00 160.00   58
  4  \w    104.00 156.00   0.50   16.00    --  111.00  98.00 -92.00  104
  5  \w   -116.00  -3.00   0.50    4.00    --  -38.50 -19.00 150.00  226
  6  \w    -27.00  65.00   0.50    4.00    --   42.50 -38.00  60.00  184
  7  \w     24.00 107.00   0.50    4.00    --   42.50  57.00  30.00  166
  8  \w     53.00  98.00   0.50    4.00    --   42.50-125.00  60.00   90
  9  \w     41.00 135.00   0.50   16.00    --  111.00 -61.00  60.00  188
 10  \w     47.00  74.00   0.50   16.00    --  111.00 -30.00 -90.00   54
 11  \w     99.00 132.00   0.50   16.00    --  111.00 125.00 -30.00   66
 12  \w     85.00 112.00   0.50   16.00    --  111.00-125.00 150.00   54
 13  \w     50.00  80.00   0.50   16.00    --  111.00-125.00 -60.00   60
 14  \w     30.00 107.00   0.50   16.00    --  111.00 -94.00 -60.00  154
 15  \w     39.00 107.00   0.50   16.00    --  111.00 -94.00-150.00  136
 16  \w     94.00 178.00   0.50   16.00    --  111.00  30.00  90.00  168
 17  \w     32.00 107.00   0.50   16.00    --  111.00 -94.00   0.00  150
 18  \w     97.00 148.00   0.50   16.00    --  111.00 125.00   0.00  102
 19  \w     45.00  70.00   0.50   16.00    --  111.00-125.00 150.00   50
 20  \w     71.00 105.00   0.50   16.00    --  111.00 -94.00-180.00   68
 21  \w     39.00  66.00   0.50   16.00    --  111.00 -94.00-180.00   54
 22  \w     50.00  77.00   0.50   16.00    --  111.00 -94.00  30.00   54
 23  \w     80.00 107.00   0.50   16.00    --  111.00 -94.00  30.00   54
 24  \w     30.00  74.00   0.50   16.00    --  111.00 -94.00 -30.00   88
 25  \w     77.00 104.00   0.50   16.00    --  111.00  15.00-120.00   54
 26  \w    124.00 167.00   0.50   16.00    --  111.00  15.00-120.00   86
 27  \w     77.00 135.00   0.50   16.00    --  111.00 -30.00 -90.00  116
 28  \w     48.00  77.00   0.50   16.00    --  111.00-125.00 120.00   58
 29  \w     46.00  73.00   0.50   16.00    --  111.00 -94.00  60.00   54
 30  \w     74.00 107.00   0.50   16.00    --  111.00 -94.00  60.00   66
 31  \w    106.00 136.00   0.50   16.00    --  111.00  30.00 120.00   60
 32  \w    150.00 178.00   0.50   16.00    --  111.00  30.00 120.00   56
 33  \w     90.00 178.00   0.50   16.00    --  111.00  45.00 150.00  176
 34  \w     72.00 107.00   0.50   16.00    --  111.00 -99.00 -18.78   70
 35  \w     35.00 106.00   0.50   16.00    --  111.00 -94.00-120.00  142
 36  \w    107.00 132.00   0.50   16.00    --  111.00 125.00  30.00   50
 37  \w    141.00 166.00   0.50   16.00    --  111.00 125.00  30.00   50
 38  \w     68.00  93.00   0.50   16.00    --  111.00-125.00-180.00   50
 39  \w    108.00 137.00   0.50   16.00    --  111.00 -61.00 -60.00   58
;
_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      0.0194494000
_diffrn_orient_matrix_UB_12      -0.0322021000
_diffrn_orient_matrix_UB_13      -0.0335906000
_diffrn_orient_matrix_UB_21      -0.0448567000
_diffrn_orient_matrix_UB_22      -0.0218524000
_diffrn_orient_matrix_UB_23      -0.0226140000
_diffrn_orient_matrix_UB_31      -0.0031623000
_diffrn_orient_matrix_UB_32      0.1116398000
_diffrn_orient_matrix_UB_33      -0.0141217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            170311
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.937
_diffrn_reflns_theta_min         2.459
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.463
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.222
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.097
_refine_diff_density_max         3.751
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1794
_refine_ls_number_reflns         31455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+127.0598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30867
_reflns_number_total             31455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           jjw1252
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_cell_volume        15000.89(14)
_cod_database_code               7706617
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C68H96N8O16P4U
_shelx_estimated_absorpt_t_max   0.531
_shelx_estimated_absorpt_t_min   0.149
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
2.a Ternary CH refined with riding coordinates:
 C12A(H12A), C15A(H15A), C29A(H29A), C32A(H32A), C46A(H46A), C49A(H49A),
 C63A(H63A), C66A(H66A), C12B(H12B), C15B(H15B), C29B(H29B), C32B(H32B),
 C46B(H46B), C49B(H49B), C63B(H63B), C66B(H66B)
2.b Me refined with riding coordinates:
 C38A(H38A,H38B,H38C)
2.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C7A(H7A), C9A(H9A), C10A(H10A), C23A(H23A), C24A(H24A), C26A(H26A),
 C27A(H27A), C40A(H40A), C41A(H41A), C43A(H43A), C44A(H44A), C57A(H57A),
 C58A(H58A), C60A(H60A), C61A(H61A), C6B(H6B), C7B(H7B), C9B(H9B), C10B(H10B),
 C23B(H23B), C24B(H24B), C26B(H26B), C27B(H27B), C40B(H40B), C41B(H41B),
 C43B(H43B), C44B(H44B), C57B(H57B), C58B(H58B), C60B(H60B), C61B(H61B)
2.d Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C11A(H11A,H11B,H11C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C21A(H21A,H21B,H21C),
 C28A(H28A,H28B,H28C), C30A(H30A,H30B,H30C), C31A(H31A,H31B,H31C), C33A(H33A,
 H33B,H33C), C34A(H34A,H34B,H34C), C45A(H45A,H45B,H45C), C47A(H47A,H47B,H47C),
 C48A(H48A,H48B,H48C), C50A(H50A,H50B,H50C), C51A(H51A,H51B,H51C), C55A(H55A,
 H55B,H55C), C62A(H62A,H62B,H62C), C64A(H64A,H64B,H64C), C65A(H65A,H65B,H65C),
 C67A(H67A,H67B,H67C), C68A(H68A,H68B,H68C), C4B(H4BA,H4BB,H4BC), C11B(H11D,
 H11E,H11F), C13B(H13D,H13E,H13F), C14B(H14E,H14F,H14D), C16B(H16D,H16E,H16F),
 C17B(H17D,H17E,H17F), C21B(H21E,H21D,H21F), C28B(H28D,H28E,H28F), C30B(H30D,
 H30E,H30F), C31B(H31D,H31E,H31F), C33B(H33D,H33E,H33F), C34B(H34F,H34D,H34E),
 C38B(H38D,H38E,H38F), C45B(H45D,H45E,H45F), C47B(H47D,H47E,H47F), C48B(H48D,
 H48E,H48F), C50B(H50D,H50E,H50F), C51B(H51D,H51E,H51F), C55B(H55D,H55E,H55F),
 C62B(H62E,H62F,H62D), C64B(H64E,H64F,H64D), C65B(H65D,H65E,H65F), C67B(H67E,
 H67F,H67D), C68B(H68E,H68D,H68F)
;
_shelx_res_checksum              94842
_shelx_hkl_checksum              24835
_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 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.627