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_4322703
_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
_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                82.810(2)
_cell_angle_beta                 74.120(2)
_cell_angle_gamma                63.054(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9927(5)
_cell_length_b                   14.4838(6)
_cell_length_c                   18.7195(6)
_cell_measurement_reflns_used    8681
_cell_measurement_temperature    20
_cell_measurement_theta_max      56
_cell_measurement_theta_min      2
_cell_volume                     3252.9(2)
_computing_cell_refinement
;
Special software of the Institut Laue Langevin in Grenoble
;
_computing_data_collection
;
Special software of the Institut Laue Langevin in Grenoble
;
_computing_data_reduction
;
Special software of the Institut Laue Langevin in Grenoble
;
_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
;
Starting model for the refinement was used from the corresponding
X-ray diffraction experiment.
;
_diffrn_ambient_temperature      20
_diffrn_measurement_device       'D19 in Grenoble'
_diffrn_measurement_method       'area detector technology'
_diffrn_radiation_monochromator  'Experimental setup of D19 in Grenoble'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           'thermal neutrons'
_diffrn_radiation_wavelength     1.5394
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8681
_diffrn_reflns_theta_max         55.68
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.20
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            ' brown '
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_size_max          2.50
_exptl_crystal_size_mid          2.34
_exptl_crystal_size_min          1.00
_refine_diff_density_max         0.93
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.1781
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         4596
_refine_ls_R_factor_obs          0.0748
_refine_ls_shift/esd_max         0.002626
_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         0.0700
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          4596
_reflns_number_total             5401
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic970891k_1.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        3254.18
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C57 H53 B1 D21 F15 N3 Si6 U1 '
_cod_database_code               4322703
_cod_database_fobs_code          4322703