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_4336497
_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         'C45 H51 Co1 I2 N3 P3 U1'
_chemical_formula_sum            'C45 H51 Co I2 N3 P3 U'
_chemical_formula_weight         1277.62
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.518(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2544(10)
_cell_length_b                   12.5472(6)
_cell_length_c                   18.9608(10)
_cell_measurement_reflns_used    7823
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      63
_cell_measurement_theta_min      4
_cell_volume                     4958.6(4)
_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
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9640
_diffrn_measured_fraction_theta_max 0.9640
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40853
_diffrn_reflns_theta_full        63.4
_diffrn_reflns_theta_max         63.41
_diffrn_reflns_theta_min         4.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.671
_exptl_absorpt_correction_T_max  0.6355
_exptl_absorpt_correction_T_min  0.4384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski &amp; Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         2.72
_refine_diff_density_min         -1.95
_refine_ls_extinction_coef       0.51E-04
_refine_ls_extinction_method     'SHELXL97 (Sheldrick 2008)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7803
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.100
_refine_ls_R_factor_gt           0.085
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+144.3734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.175
_refine_ls_wR_factor_ref         0.183
_reflns_number_gt                6368
_reflns_number_total             7803
_reflns_threshold_expression     &gt;2.0\s(I)
_cod_data_source_file            ic402343q_si_002_1.cif
_cod_data_source_block           CT6
_cod_depositor_comments
;
 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-01-20

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_formula_sum        'C45 H51 Co1 I2 N3 P3 U1'
_cod_database_code               4336497