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_7706616
_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, C H2 Cl2'
_chemical_formula_sum            'C69 H98 Cl2 N8 O16 P4 U'
_chemical_formula_weight         1728.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-28
_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                 92.9022(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.69468(8)
_cell_length_b                   24.32535(12)
_cell_length_c                   23.65863(10)
_cell_measurement_reflns_used    52319
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.7280
_cell_measurement_theta_min      2.5870
_cell_volume                     7871.24(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 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -78.00  14.00   0.50    5.00    --  -38.50  98.00 -79.00  184
  2  \w     37.00  64.00   0.50    5.00    --   42.62 -98.00 173.00   54
  3  \w    117.00 142.00   0.50   20.00    --  111.00  98.00 -79.00   50
  4  \w     60.00 106.00   0.50   20.00    --  111.00 -98.00 173.00   92
  5  \w    -82.00  -6.00   0.50    5.00    --  -38.50 125.00  60.00  152
  6  \w   -109.00 -40.00   0.50    5.00    --  -38.50 -38.00-150.00  138
  7  \w      2.00  27.00   0.50    5.00    --  -38.50  38.00  90.00   50
  8  \w   -111.00 -18.00   0.50    5.00    --  -38.50 -38.00 120.00  186
  9  \w     16.00  81.00   0.50    5.00    --   42.62  57.00  60.00  130
 10  \w     33.00  78.00   0.50   20.00    --  111.00 -94.00-150.00   90
 11  \w     42.00  68.00   0.50   20.00    --  111.00 -61.00 -30.00   52
 12  \w     87.00 178.00   0.50   20.00    --  111.00  30.00   0.00  182
 13  \w     97.00 169.00   0.50   20.00    --  111.00 125.00-120.00  144
 14  \w     80.00 107.00   0.50   20.00    --  111.00 -94.00 -60.00   54
 15  \w    131.00 175.00   0.50   20.00    --  111.00  77.00 -60.00   88
 16  \w     84.00 112.00   0.50   20.00    --  111.00 -61.00 -30.00   56
 17  \w     80.00 107.00   0.50   20.00    --  111.00 -94.00-120.00   54
 18  \w     68.00 139.00   0.50   20.00    --  111.00  15.00 -60.00  142
 19  \w    138.00 172.00   0.50   20.00    --  111.00  77.00-120.00   68
 20  \w     45.00 112.00   0.50   20.00    --  111.00-125.00-180.00  134
 21  \w     42.00  69.00   0.50   20.00    --  111.00-125.00  30.00   54
 22  \w     46.00  93.00   0.50   20.00    --  111.00-125.00   0.00   94
 23  \w    103.00 130.00   0.50   20.00    --  111.00  77.00-150.00   54
 24  \w    136.00 177.00   0.50   20.00    --  111.00  77.00-150.00   82
 25  \w     32.00  72.00   0.50   20.00    --  111.00 -94.00  30.00   80
 26  \w     80.00 107.00   0.50   20.00    --  111.00 -94.00  30.00   54
 27  \w     64.00  91.00   0.50   20.00    --  111.00-125.00 -60.00   54
 28  \w     84.00 111.00   0.50   20.00    --  111.00 -45.00   0.00   54
 29  \w     35.00  80.00   0.50   20.00    --  111.00 -15.00 -30.00   90
 30  \w     94.00 136.00   0.50   20.00    --  111.00 -15.00 -30.00   84
 31  \w     40.00  77.00   0.50   20.00    --  111.00 -45.00   0.00   74
 32  \w    113.00 155.00   0.50   20.00    --  111.00 125.00 -60.00   84
 33  \w     40.00  65.00   0.50   20.00    --  111.00-125.00 -30.00   50
 34  \w     74.00 112.00   0.50   20.00    --  111.00-125.00 -30.00   76
 35  \w    145.00 170.00   0.50   20.00    --  111.00  15.00 -60.00   50
 36  \w     58.00 108.00   0.50   20.00    --  111.00-105.00  94.89  100
 37  \w     42.00  69.00   0.50   20.00    --  111.00-125.00 -90.00   54
 38  \w     76.00 112.00   0.50   20.00    --  111.00-125.00 -90.00   72
 39  \w    108.00 135.00   0.50   20.00    --  111.00  77.00-120.00   54
 40  \w     72.00 110.00   0.50   20.00    --  111.00-125.00  30.00   76
 41  \w     80.00 107.00   0.50   20.00    --  111.00 -94.00   0.00   54
 42  \w     40.00 134.00   0.50   20.00    --  111.00 -45.00-180.00  188
;
_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      -0.0784432000
_diffrn_orient_matrix_UB_12      -0.0406234000
_diffrn_orient_matrix_UB_13      -0.0232503000
_diffrn_orient_matrix_UB_21      0.0795901000
_diffrn_orient_matrix_UB_22      -0.0438414000
_diffrn_orient_matrix_UB_23      -0.0073698000
_diffrn_orient_matrix_UB_31      -0.0145142000
_diffrn_orient_matrix_UB_32      -0.0209360000
_diffrn_orient_matrix_UB_33      0.0604313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            92948
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.024
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.751
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.522
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.284
_refine_diff_density_min         -2.532
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         16496
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0670P)^2^+10.2003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15673
_reflns_number_total             16496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           jjw1251
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_database_code               7706616
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C69H98Cl2N8O16P4U
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34B)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=
 Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(H46A)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48D)=
 Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(H46)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48A)=Sof(H48A)=
 Sof(H48B)=Sof(H48C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C29(H29), C46(H46), C46(H46A), C49(H49), C63(H63),
 C66(H66), C32A(H32A), C32B(H32B)
4.b Secondary CH2 refined with riding coordinates:
 C69(H69B,H69A)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C23(H23), C24(H24), C26(H26), C27(H27),
 C40(H40), C41(H41), C43(H43), C44(H44), C57(H57), C58(H58), C60(H60), C61(H61)
4.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), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C),
 C45(H45A,H45B,H45C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C55(H55A,H55B,
 H55C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C33A(H33D,H33E,H33F), C34A(H34A,H34B,H34C),
 C47A(H47A,H47B,H47C), C48A(H48A,H48B,H48C), C33B(H33A,H33B,H33C), C34B(H34D,
 H34E,H34F), C47B(H47D,H47E,H47F), C48B(H48D,H48E,H48F)
;
_shelx_res_checksum              32522
_shelx_hkl_checksum              59923
_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 3.803
_oxdiff_exptl_absorpt_empirical_full_min 0.687