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_7706615
_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_absolute_configuration ad
_chemical_formula_moiety         'C68 H97 Ce N8 O16 P4, C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C74 H110 Ce N9 O17 P4'
_chemical_formula_weight         1661.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-27
_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                 106.0730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.16990(10)
_cell_length_b                   18.44880(10)
_cell_length_c                   17.90400(10)
_cell_measurement_reflns_used    33246
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5680
_cell_measurement_theta_min      2.5600
_cell_volume                     4180.07(5)
_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      100.00(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 0.993
_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    -65.00  11.00   0.50    3.00    --  -38.50  96.00  48.00  152
  2  \w    153.00 178.00   0.50   12.00    --  111.00  96.00  48.00   50
  3  \w     80.00 106.00   0.50   12.00    --  111.00 -96.00 -60.00   52
  4  \w    105.00 135.00   0.50   12.00    --  111.00  96.00  48.00   60
  5  \w   -105.00 -28.00   0.50    3.00    --  -38.50 -38.00-180.00  154
  6  \w   -108.00 -17.00   0.50    3.00    --  -38.50 -57.00 -90.00  182
  7  \w      6.00  56.00   0.50    3.00    --   42.50 -99.00   0.00  100
  8  \w     23.00  50.00   0.50    3.00    --   42.50 -96.00 -60.00   54
  9  \w     30.00 103.00   0.50    3.00    --   42.50  38.00-180.00  146
 10  \w     55.00  98.00   0.50    3.00    --   42.50-125.00-180.00   86
 11  \w     32.00 106.00   0.50   12.00    --  111.00 -94.00-150.00  148
 12  \w    103.00 177.00   0.50   12.00    --  111.00  77.00   0.00  148
 13  \w     84.00 111.00   0.50   12.00    --  111.00 -30.00  60.00   54
 14  \w     87.00 151.00   0.50   12.00    --  111.00  45.00 -30.00  128
 15  \w     90.00 117.00   0.50   12.00    --  111.00 -61.00 120.00   54
 16  \w     79.00 110.00   0.50   12.00    --  111.00-125.00  60.00   62
 17  \w     42.00 137.00   0.50   12.00    --  111.00 -61.00-150.00  190
 18  \w    113.00 177.00   0.50   12.00    --  111.00  77.00 -30.00  128
 19  \w    104.00 177.00   0.50   12.00    --  111.00  77.00  30.00  146
 20  \w     52.00 107.00   0.50   12.00    --  111.00 -94.00 120.00  110
 21  \w     82.00 107.00   0.50   12.00    --  111.00-101.00-101.05   50
 22  \w     59.00  86.00   0.50   12.00    --  111.00-125.00  90.00   54
 23  \w     73.00 104.00   0.50   12.00    --  111.00 -94.00-180.00   62
 24  \w     59.00 106.00   0.50   12.00    --  111.00 -94.00   0.00   94
 25  \w    106.00 146.00   0.50   12.00    --  111.00  15.00-120.00   80
 26  \w    135.00 178.00   0.50   12.00    --  111.00  30.00 -60.00   86
 27  \w     30.00  76.00   0.50   12.00    --  111.00 -94.00  90.00   92
 28  \w     77.00 107.00   0.50   12.00    --  111.00 -94.00  90.00   60
 29  \w    102.00 132.00   0.50   12.00    --  111.00  30.00 -60.00   60
 30  \w     40.00  90.00   0.50   12.00    --  111.00-125.00-180.00  100
 31  \w     86.00 131.00   0.50   12.00    --  111.00 -77.00-120.00   90
 32  \w     31.00 106.00   0.50   12.00    --  111.00 -94.00  60.00  150
 33  \w     83.00 153.00   0.50   12.00    --  111.00  61.00  90.00  140
 34  \w     42.00 112.00   0.50   12.00    --  111.00-125.00-150.00  140
 35  \w     46.00 127.00   0.50   12.00    --  111.00 -45.00 -60.00  162
 36  \w     36.00  69.00   0.50   12.00    --  111.00 -30.00  60.00   66
;
_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      0.0431034000
_diffrn_orient_matrix_UB_12      0.0779174000
_diffrn_orient_matrix_UB_13      0.0035023000
_diffrn_orient_matrix_UB_21      0.0490780000
_diffrn_orient_matrix_UB_22      -0.0077575000
_diffrn_orient_matrix_UB_23      0.0883752000
_diffrn_orient_matrix_UB_31      0.1027042000
_diffrn_orient_matrix_UB_32      -0.0289567000
_diffrn_orient_matrix_UB_33      -0.0142778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49599
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.835
_diffrn_reflns_theta_min         2.568
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88435
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1742
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 6542 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0114(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         15854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0746P)^2^+0.9839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.796
_reflns_number_gt                15680
_reflns_number_total             15854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           jjw1236
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_database_code               7706615
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O P S Ce Cl'
_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, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C29(H29), C32(H32), C46(H46), C49(H49), C63(H63), C66(H66)
2.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C73(H73A,H73B)
2.c Aromatic/amide H refined with riding coordinates:
 N8(H8), 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)
2.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), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), 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), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              17927
_shelx_hkl_checksum              21380
_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 1.717
_oxdiff_exptl_absorpt_empirical_full_min 0.802