Tris(phosphinoamide)-Supported Uranium-Cobalt Heterobimetallic Complexes Featuring Co → U Dative Interactions
J. Wesley Napoline; Steven J. Kraft; Ellen M. Matson; Phillip E. Fanwick; Suzanne C. Bart; Christine M. Thomas; Inorganic Chemistry 52 (2013) 12170–12177; doi:10.1021/ic402343q

data_4336498
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Fanwick, Phillip E.'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Tris(phosphinoamide)-Supported Uranium-Cobalt Heterobimetallic Complexes
 Featuring Co \\rightarrow U Dative Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12170
_journal_page_last               12177
_journal_paper_doi               10.1021/ic402343q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C60 H68 N4 P4 U1,2(C4 H10 O1)'
_chemical_formula_sum            'C68 H88 N4 O2 P4 U'
_chemical_formula_weight         1355.41
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 126.680(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6106(8)
_cell_length_b                   23.0882(9)
_cell_length_c                   16.9302(6)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     6461.1(5)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 direct methods (SIR2011, Burla et al., in press)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9590
_diffrn_measured_fraction_theta_max 0.9590
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not cusp 
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            58949
_diffrn_reflns_theta_full        72.4
_diffrn_reflns_theta_max         72.38
_diffrn_reflns_theta_min         3.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.357
_exptl_absorpt_correction_T_max  0.4336
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski &amp; Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.70
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+22.0655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.162
_refine_ls_wR_factor_ref         0.164
_reflns_number_gt                5885
_reflns_number_total             6129
_reflns_threshold_expression     &gt;2.0\s(I)
_cod_data_source_file            ic402343q_si_002_2.cif
_cod_data_source_block           CT1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        6461.1(4)
_cod_original_formula_sum        'C68 H88 N4 O2 P4 U1'
_cod_database_code               4336498