Syntheses of the Uranium Complexes [U{N(SiMe3)2}2{N(SiMe3)(SiMe2CH2B(C6F5)3)}] and [U{C(Ph)(NSiMe3)2}2{μ3-BH4}2]. Determination of Hydrogen Positions by Single-Crystal X-ray and Neutron Diffraction
Matthias Müller; V. Cliff Williams; Linda H. Doerrer; Michael A. Leech; Sax A. Mason; Malcolm L. H. Green; Keith Prout; Inorganic Chemistry 37 (1998) 1315–1323; doi:10.1021/ic970891k

data_4322705
_publ_contact_author
;
Linda H. Doerrer
Inorganic Chemistry Laboratory
University of Oxford
South Parks Road
Oxford OX1 3QR, UK
;
_publ_contact_author_email       ' linda.doerrer@chem.ox.ac.uk '
_publ_contact_author_fax         ' 01865 272 690 '
_publ_contact_author_phone       ' 01865 272 675 '
_publ_section_title
;
 Syntheses of the Uranium Complexes
 [U{N(SiMe3)2}2{N(SiMe3)(SiMe2CH2B(C6F5)3)}] and
 [U{C(Ph)(NSiMe3)2}2{\m3-BH4}2]. Determination of Hydrogen Positions by
 Single-Crystal X-ray and Neutron Diffraction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1315
_journal_page_last               1323
_journal_paper_doi               10.1021/ic970891k
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
synthesis
;
_chemical_formula_moiety         ' C36 H53 B1 F15 N3 Si6 U1, 3.5(C6 D6) '
_chemical_formula_sum            'C57 H53 B D21 F15 N3 Si6 U'
_chemical_formula_weight         1524.69
_chemical_name_systematic
;
 unknown
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             97-06-04
_audit_creation_method           CRYSTALS
_cell_angle_alpha                82.898(1)
_cell_angle_beta                 74.415(1)
_cell_angle_gamma                62.919(1)
_cell_formula_units_Z            2
_cell_length_a                   14.064(1)
_cell_length_b                   14.496(1)
_cell_length_c                   18.759(1)
_cell_measurement_reflns_used    38829
_cell_measurement_temperature    90
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     3279.9(4)
_computing_cell_refinement
'Denzo, Scalepack (Z. Otwinowski, W. Minor 1996)'
_computing_data_collection
'DIP2020 images plate software (Enraf-Nonius, 1989)'
_computing_data_reduction
'Denzo, Scalepack (Z. Otwinowski, W. Minor 1996)'
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      90
_diffrn_measurement_device       '  Enraf-nonius DIP2020 image plate '
_diffrn_measurement_method       'image plate technology '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38829
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.53
_exptl_absorpt_correction_T_max  1.27
_exptl_absorpt_correction_T_min  1.01
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' brown '
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' cubic block '
_exptl_crystal_F_000             1486.09
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.11
_refine_diff_density_min         -1.69
_refine_ls_extinction_coef       333.1(128)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         12188
_refine_ls_R_factor_obs          0.0239
_refine_ls_shift/esd_max         0.014806
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0273
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_observed          12188
_reflns_number_total             12827
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic970891k_3.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3279.93
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C57 H53 B1 D21 F15 N3 Si6 U1 '
_cod_database_code               4322705
_cod_database_fobs_code          4322705
_exptl_absorpt_correction_details
;
by scaling and merging equivalent reflections from
different frames, close to multi-scan
;