Synthesis and Structural Characterization of Unprecedented Bis-Asymmetric Heteroscorpionate U(III) Complexes: [U{κ3-H2B(pztBu,Me)(pzMe,tBu)}2I] and [U{κ3-H2B(pztBu,Me)(pzMe2)}2I]
Leonor Maria; Ângela Domingos; Isabel Santos; Inorganic Chemistry 42 (2003) 3323–3330; doi:10.1021/ic026210p

data_4313641
_publ_section_title
;
 Synthesis and Structural Characterization of Unprecedented Bis-Asymmetric
 Heteroscorpionate U(III) Complexes: [U{\k3-H2B(pztBu,Me)(pzMe,tBu)}2I]
 and [U{\k3-H2B(pztBu,Me)(pzMe2)}2I]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3323
_journal_page_last               3330
_journal_paper_doi               10.1021/ic026210p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural     '[UI{k3-BptBu,Me)2}(HpztBu,Me)(u-I)]2.2C7H8'
_chemical_formula_sum            'C62 H100 B2 I4 N12 U2'
_chemical_formula_weight         2018.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0500(10)
_cell_length_b                   20.460(4)
_cell_length_c                   17.361(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      7.6
_cell_volume                     3918.0(10)
_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-3 (Farrugia,1997)'
_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\qscans
_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  0.0956
_diffrn_reflns_av_sigmaI/netI    0.1758
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6376
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        10.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.745
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.5041
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.101
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.292
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.2296
_refine_ls_R_factor_obs          0.0988
_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^)+(0.0855P)^2^+43.1541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3069
_refine_ls_wR_factor_obs         0.1834
_reflns_number_observed          2816
_reflns_number_total             6148
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026210psi20030121_040124_3.cif
_cod_data_source_block           xul2i
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+43.1541P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+43.1541P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313641