Solvent-Free Organometallic Reactivity: Synthesis of Hydride and Carboxylate Complexes of Uranium and Yttrium from Gas/Solid Reactions
Webster, Christopher L.; Ziller, Joseph W.; Evans, William J.; Organometallics 33 (2014) 433–; doi:10.1021/om401122d

data_4082522
_publ_section_title
;
 Solvent-Free Organometallic Reactivity: Synthesis of Hydride and
 Carboxylate Complexes of Uranium and Yttrium from Gas/Solid Reactions
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              433
_journal_paper_doi               10.1021/om401122d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C47 H70 Y2'
_chemical_formula_weight         812.85
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.6476(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9754(15)
_cell_length_b                   31.177(4)
_cell_length_c                   12.5004(17)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.29
_cell_volume                     4216.9(10)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2012.4-0, 2012'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      83(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            49412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_correction_T_min  0.2027
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rod
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.826
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         10238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.1574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7627
_reflns_number_total             10238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401122d_si_001.cif
_cod_data_source_block           clw45
_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 
;
_cod_database_code               4082522
_shelx_estimated_absorpt_t_min   0.208
_shelx_estimated_absorpt_t_max   0.741
_shelxl_version_number           2013-3
_shelx_res_checksum              54830
_shelx_hkl_checksum              28404