Half- and Mixed-Sandwich Uranium Permethylpentalene Compounds
Chadwick, F. Mark; O’Hare, Dermot M.; Organometallics 33 (2014) 3768–; doi:10.1021/om500474h

data_4083994
_publ_section_title
;
 Half- and Mixed-Sandwich Uranium Permethylpentalene Compounds
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3768
_journal_paper_doi               10.1021/om500474h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H49 Cl2 Li1 N2 U1'
_chemical_formula_sum            'C30 H49 Cl2 Li N2 U'
_chemical_formula_weight         753.61
_chemical_melting_point          ?
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-06-11
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 104.1914(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   10.62130(10)
_cell_length_b                   43.4930(5)
_cell_length_c                   21.1430(3)
_cell_measurement_reflns_used    14573
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     9469.0(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49711
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         5.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.332
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.59
_refine_diff_density_min         -2.92
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9581
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         20381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.0021221
_refine_ls_shift/su_mean         0.0000126
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 6.83 7.05 2.89 0.449 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1236
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1233
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              56
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                13905
_reflns_number_total             20391
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.20
_oxford_diffrn_Wilson_scale      463.15
_oxford_refine_ls_r_factor_ref   0.1029
_oxford_refine_ls_scale          0.051613(4)
_oxford_reflns_number_all        20391
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '100fmc11 At 19:45 on 11/ 6'
_cod_data_source_file            om500474h_si_002.cif
_cod_data_source_block           UPnstarCpstarCl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 4083993--4083994.cif.

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 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C30 H49 Cl2 Li1 N2 U1'
_cod_database_code               4083994
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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