Synthesis and structure of uranium(III) complexes with dihydrobis(pyrazolyl)borates
Maria, Leonor; Campello, Maria Paula; Domingos, Ângela; Santos, Isabel; Andersen, Richard; Journal of the Chemical Society, Dalton Transactions  (1999) 2015–; doi:10.1039/a900744j

data_7702374
_publ_section_title
;
 Synthesis and structure of uranium(III) complexes with
 dihydrobis(pyrazolyl)borates
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2015
_journal_paper_doi               10.1039/a900744j
_journal_year                    1999
_chemical_formula_structural     '[U{H2B(3tBu,5Me-pz)2}I2(THF)2].THF'
_chemical_formula_sum            'C28 H52 B I2 N4 O3 U'
_chemical_formula_weight         995.38
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3860(10)
_cell_length_b                   13.1150(10)
_cell_length_c                   26.556(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      7.7
_cell_volume                     3617.3(5)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MOLEN(Fair,1990)
_computing_molecular_graphics    ORTEP(Johnson,1976)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4-Enraf Nonius'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1496
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5512
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count '100 reflections'
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.225
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.7705
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.656
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_obs          0.0724
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+35.9195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1997
_refine_ls_wR_factor_obs         0.1003
_reflns_number_observed          2961
_reflns_number_total             5247
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900744j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+35.9195P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+35.9195P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7702374