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_7706614
_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         'C53 H75 Ce N7 O12 P3'
_chemical_formula_sum            'C53 H75 Ce N7 O12 P3'
_chemical_formula_weight         1235.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-26
_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                91.504(2)
_cell_angle_beta                 90.766(2)
_cell_angle_gamma                111.160(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6391(3)
_cell_length_b                   13.3055(3)
_cell_length_c                   20.5728(3)
_cell_measurement_reflns_used    18881
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7693
_cell_measurement_theta_min      3.5632
_cell_volume                     2969.26(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -83.00   4.00   0.50    3.00    --  -38.50  15.00 -20.00  174
  2  \w   -113.00   7.00   0.50    3.00    --  -38.50 -15.00 169.00  240
  3  \w     25.00  76.00   0.50    3.00    --   42.25 -15.00 169.00  102
  4  \w     67.00  97.00   0.50    3.00    --   42.25  15.00 -20.00   60
  5  \w     98.00 123.00   0.50   12.00    --  111.00  15.00 -20.00   50
  6  \w     34.00 105.00   0.50   12.00    --  111.00 -15.00 169.00  142
  7  \w     10.00  36.00   0.50    3.00    --  -38.50  15.00 -20.00   52
  8  \w   -107.00 -75.00   0.50    3.00    --  -38.50 -64.00 172.70   64
  9  \w    -82.00  -6.00   0.50    3.00    --  -38.50 125.00 120.00  152
 10  \w   -106.00 -64.00   0.50    3.00    --  -38.50 -57.00 -30.00   84
 11  \w    -87.00  -6.00   0.50    3.00    --  -38.50 125.00 -90.00  162
 12  \w    -38.00 -10.00   0.50    3.00    --  -38.50 -64.00 172.70   56
 13  \w    -59.00 -13.00   0.50    3.00    --  -38.50 -57.00 -30.00   92
 14  \w     20.00  69.00   0.50    3.00    --   42.25  38.00  30.00   98
 15  \w     27.00  83.00   0.50    3.00    --   42.25-125.00 120.00  112
 16  \w     13.00  41.00   0.50    3.00    --   46.00  82.00-102.12   56
 17  \w     13.00  38.00   0.50    3.00    --   46.00  82.00 123.28   50
 18  \w     14.00  39.00   0.50    3.00    --   46.00  79.00-163.46   50
 19  \w     14.00  39.00   0.50    3.00    --   46.00  80.00  59.38   50
 20  \w     14.00  39.00   0.50    3.00    --   46.00  78.00 -17.45   50
 21  \w     82.00 110.00   0.50    3.00    --   58.00  72.00 120.70   56
 22  \w     29.00  67.00   0.50    3.00    --   58.00  73.00  76.17   76
 23  \w     28.00  56.00   0.50    3.00    --   58.00  72.00 120.70   56
 24  \w     32.00  75.00   0.50    3.00    --   62.00  73.00-100.05   86
 25  \w     32.00  58.00   0.50    3.00    --   62.00  73.00-161.45   52
 26  \w    106.00 134.00   0.50    3.00    --   62.00  73.00-127.42   56
 27  \w     31.00  59.00   0.50    3.00    --   62.00  74.00 -27.02   56
 28  \w     31.00  59.00   0.50    3.00    --   62.00  74.00 148.34   56
 29  \w     33.00  78.00   0.50    3.00    --   62.00  73.00-127.42   90
 30  \w     36.00  80.00   0.50    3.00    --   66.00  71.00  41.06   88
 31  \w     36.00  64.00   0.50    3.00    --   66.00  73.00  -4.72   56
 32  \w     41.00  68.00   0.50    3.00    --   70.00  67.00 159.76   54
 33  \w     43.00  75.00   0.50    3.00    --   70.00  59.00 103.77   64
 34  \w     44.00  72.00   0.50    3.00    --   74.00  72.00 -25.83   56
 35  \w     47.00 122.00   0.50    3.00    --   74.00  64.00 115.82  150
 36  \w     43.00  71.00   0.50    3.00    --   74.00  74.00 -87.12   56
 37  \w     45.00 117.00   0.50    3.00    --   74.00  71.00 -61.41  144
 38  \w     51.00  76.00   0.50   12.00    --   78.00  64.00-147.08   50
 39  \w     49.00  75.00   0.50   12.00    --   78.00  73.00-131.39   52
 40  \w     48.00 102.00   0.50   12.00    --   78.00  70.00   1.29  108
 41  \w    116.00 144.00   0.50   12.00    --   82.00  68.00 178.94   56
 42  \w     53.00  82.00   0.50   12.00    --   82.00  68.00 178.94   58
 43  \w     52.00  82.00   0.50   12.00    --   82.00  71.00 156.83   60
 44  \w     59.00  89.00   0.50   12.00    --   86.00  57.00 -30.42   60
 45  \w     61.00  96.00   0.50   12.00    --   90.00  67.00  19.73   70
 46  \w     61.00  89.00   0.50   12.00    --   90.00  71.00 -99.07   56
 47  \w    125.00 153.00   0.50   12.00    --   90.00  67.00  19.73   56
 48  \w     71.00  99.00   0.50   12.00    --   98.00  58.00-119.62   56
 49  \w     73.00 101.00   0.50   12.00    --   98.00  55.00 -24.72   56
 50  \w     71.00 102.00   0.50   12.00    --  102.00  74.00   5.78   62
 51  \w     76.00 104.00   0.50   12.00    --  106.00  71.00 155.75   56
 52  \w     83.00 155.00   0.50   12.00    --  111.00  61.00  60.00  144
 53  \w     83.00 173.00   0.50   12.00    --  111.00  61.00-150.00  180
 54  \w     83.00 167.00   0.50   12.00    --  111.00  61.00 -30.00  168
 55  \w     38.00  76.00   0.50   12.00    --  111.00 -94.00 -60.00   76
 56  \w     83.00 174.00   0.50   12.00    --  111.00  61.00 -90.00  182
 57  \w     83.00 177.00   0.50   12.00    --  111.00  61.00 150.00  188
 58  \w     89.00 118.00   0.50   12.00    --  111.00  45.00-150.00   58
 59  \w     83.00 160.00   0.50   12.00    --  111.00  61.00 -60.00  154
 60  \w     87.00 142.00   0.50   12.00    --  111.00  45.00 120.00  110
 61  \w     83.00 174.00   0.50   12.00    --  111.00  61.00-120.00  182
 62  \w     83.00 178.00   0.50   12.00    --  111.00  61.00  90.00  190
 63  \w     78.00 107.00   0.50   12.00    --  111.00 -94.00 -60.00   58
 64  \w     60.00 107.00   0.50   12.00    --  111.00 -94.00-150.00   94
 65  \w     39.00 107.00   0.50   12.00    --  111.00 -94.00 -90.00  136
 66  \w     82.00 107.00   0.50   12.00    --  111.00 -94.00 -30.00   50
 67  \w     40.00 129.00   0.50   12.00    --  111.00 -45.00 150.00  178
 68  \w     39.00  80.00   0.50   12.00    --  111.00 -94.00 -30.00   82
 69  \w     83.00 172.00   0.50   12.00    --  111.00  61.00 120.00  178
 70  \w    122.00 176.00   0.50   12.00    --  111.00  61.00-180.00  108
 71  \w     84.00 177.00   0.50   12.00    --  111.00  59.00  -5.41  186
 72  \w     83.00 112.00   0.50   12.00    --  111.00  61.00-180.00   58
 73  \w     66.00 107.00   0.50   12.00    --  111.00 -94.00 120.00   82
 74  \w     40.00 111.00   0.50   12.00    --  111.00-125.00-150.00  142
 75  \w     47.00 128.00   0.50   12.00    --  111.00 -45.00 -30.00  162
 76  \w     83.00 141.00   0.50   12.00    --  111.00  61.00  30.00  116
 77  \w     34.00 107.00   0.50   12.00    --  111.00 -94.00   0.00  146
 78  \w     89.00 140.00   0.50   12.00    --  111.00  45.00  60.00  102
 79  \w     70.00 133.00   0.50   12.00    --  111.00 -45.00  30.00  126
 80  \w     65.00 106.00   0.50   12.00    --  111.00 -94.00  60.00   82
;
_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      -0.1312137271
_diffrn_orient_matrix_UB_12      -0.0845002863
_diffrn_orient_matrix_UB_13      0.0042784685
_diffrn_orient_matrix_UB_21      0.0542103899
_diffrn_orient_matrix_UB_22      -0.0873408644
_diffrn_orient_matrix_UB_23      0.0139750843
_diffrn_orient_matrix_UB_31      0.0008774644
_diffrn_orient_matrix_UB_32      0.0257487022
_diffrn_orient_matrix_UB_33      0.0734924436
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69638
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.206
_diffrn_reflns_theta_min         3.564
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.208
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.405
_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    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0628P)^2^+2.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11755
_reflns_number_total             12352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           jjw1250
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_cell_volume        2969.24(12)
_cod_database_code               7706614
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C53H75CeN7O12P3
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.425
_reflns_odcompleteness_completeness 99.95
_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
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C29(H29), C32(H32), C46(H46), C49(H49)
2.b 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)
2.c 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), C53(H53A,
 H53B,H53C)
;
_shelx_res_checksum              89277
_shelx_hkl_checksum              29502
_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 1.943
_oxdiff_exptl_absorpt_empirical_full_min 0.723