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_7702376
_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{Ph2B(pz)2}3].1.5C7H8'
_chemical_formula_sum            'C64.5 H60 B3 N12 U'
_chemical_formula_weight         1273.71
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                118.957(9)
_cell_angle_beta                 92.650(11)
_cell_angle_gamma                97.356(15)
_cell_formula_units_Z            2
_cell_length_a                   13.5650(10)
_cell_length_b                   15.715(2)
_cell_length_c                   15.929(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      7.4
_cell_volume                     2923.7(6)
_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\qscan
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9397
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        4.4
_diffrn_standards_interval_count 'every 100 reflections'
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.8372
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            pink-red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.133
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.178
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_obs          0.0501
_refine_ls_shift/esd_max         -0.114
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+2.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1401
_refine_ls_wR_factor_obs         0.1161
_reflns_number_observed          6559
_reflns_number_total             8202
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900744j.txt
_cod_data_source_block           3
_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^)+(0.0728P)^2^+2.4718P] 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^)+(0.0728P)^2^+2.4718P] 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      P-1
_cod_original_formula_sum        'C64.50 H60 B3 N12 U'
_cod_database_code               7702376