Synthesis, Characterization, and High-Pressure Studies of a 3D Berkelium(III) Carboxylate Framework Material
Sperling, Joseph M.; Beck, Nicholas B.; Scheibe, Benjamin; Bai, Zhuanling; Brannon, Jacob Preston; Gomez Martinez, Daniela; Grödler, Dennis; Johnson, Jason A.; Lin, Xinsong; Rotermund, Brian Matthew; Albrecht-Schoenzart, Thomas; Chemical Communications  (2022) –; doi:10.1039/D1CC06958F

data_7129566
_publ_section_title
;
 Synthesis, Characterization, and High-Pressure Studies of a 3D
 Berkelium(III) Carboxylate Framework Material
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06958F
_journal_year                    2022
_chemical_formula_moiety         'C6 H8 Bk O10, H2 O'
_chemical_formula_sum            'C6 H10 Bk O11'
_chemical_formula_weight         507.14
_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   difmap
_audit_creation_date             2021-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2022-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.023(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4703(2)
_cell_length_b                   13.0851(3)
_cell_length_c                   9.5474(2)
_cell_measurement_reflns_used    13538
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.4640
_cell_measurement_theta_min      3.4340
_cell_volume                     1052.34(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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  33.00   0.50    7.00    --   11.88 -70.00  -8.00  188
  2  \w     -9.00  85.00   0.50    7.00    --   11.88  70.00 123.00  188
  3  \w    -12.00  25.00   0.50    7.00    --   11.88  77.00 -30.00   74
  4  \w    -12.00  25.00   0.50    7.00    --   11.88  77.00 -90.00   74
  5  \w    -25.00  36.00   0.50    7.00    --   11.88 -77.00  90.00  122
  6  \w     -7.00  22.00   0.50    7.00    --  -12.97 -99.00 -60.00   58
  7  \w     -7.00  22.00   0.50    7.00    --  -12.97 -99.00 -30.00   58
  8  \w     -7.00  22.00   0.50    7.00    --  -12.97 -99.00-180.00   58
  9  \w     -7.00  22.00   0.50    7.00    --  -12.97 -99.00-150.00   58
 10  \w    -37.00 -10.00   0.50    7.00    --  -12.97  77.00-180.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15900
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_min         3.397
_exptl_absorpt_coefficient_mu    7.805
_exptl_absorpt_correction_T_max  0.57997
_exptl_absorpt_correction_T_min  0.57195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.201
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.048
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00070(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0133
_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^)+(0.0091P)^2^+2.1952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3079
_reflns_number_total             3174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06958f2.cif
_cod_data_source_block           bk_mell_mo
_cod_database_code               7129566
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.319
_olex2_refinement_description
;
;
_shelx_res_checksum              84617
_shelx_hkl_checksum              77783
_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
;