Structural and thermodynamic investigations of Zr(BH4)4 and Hf(BH4)4 between 280 K and their decomposition temperatures
Burkmann, Konrad; Habermann, Franziska; Schumann, Erik; Kraus, Jakob; Störr, Bianca; Schmidt, Horst; Brendler, Erica; Seidel, Jürgen; Bohmhammel, Klaus; Kortus, Jens; Mertens, Florian; New Journal of Chemistry 48 (2024) 2743–2754; doi:10.1039/D3NJ05601E

data_7062966
_publ_section_title
;
 Structural and thermodynamic investigations of Zr(BH4)4 and Hf(BH4)4
 between 280 K and their decomposition temperatures
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2743
_journal_page_last               2754
_journal_paper_doi               10.1039/D3NJ05601E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'B4 H16 Zr'
_chemical_formula_weight         150.59
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   5.955(11)
_cell_length_b                   5.955(11)
_cell_length_c                   5.955(11)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    273
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      3.35
_cell_volume                     211.2(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      ' 413 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1331
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3767
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.285
_diffrn_reflns_theta_min         6.855
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.187
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       cubic
_exptl_crystal_F_000             76
_refine_diff_density_max         0.086
_refine_diff_density_min         -0.075
_refine_diff_density_rms         0.017
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.5(5)
_refine_ls_extinction_coef       0.93(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0272
_refine_ls_wR_factor_ref         0.0272
_reflns_Friedel_coverage         0.620
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                115
_reflns_number_total             115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj05601e2.cif
_cod_data_source_block           zrb4-2-273_b
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_measurement_device' was replaced with
'_diffrn_measurement_device'.

Automatic conversion script
Id: cif_correct_tags 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7062966--7062967.cif.
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_cod_original_cell_volume        211.1(12)
_cod_database_code               7062966
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              87083
_shelx_hkl_checksum              12021