Novel Lanthanocene Analogues of “Carbons Apart” Erba- and Dysprosacarboranes: Synthetic and Structural Investigation
Wang, Jianhui; Li, Shoujian; Zheng, Chong; Maguire, John A.; Hosmane, Narayan S.; Organometallics 21 (2002) 3314–; doi:10.1021/om020269m

data_4076901
_publ_section_title
;
 Novel Lanthanocene Analogues of &#x201C;Carbons Apart&#x201D; Erba- and
 Dysprosacarboranes:&#x00A0; Synthetic and Structural Investigation
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3314
_journal_paper_doi               10.1021/om020269m
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C39 H89 B12 Er Na3 Si6'
_chemical_formula_weight         1092.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.035(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.978(3)
_cell_length_b                   19.115(4)
_cell_length_c                   26.350(6)
_cell_measurement_reflns_used    845
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     6029(2)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Siemens SMART CCD  PLATFORM'
_diffrn_measurement_method       '\w scans'
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.702397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            pink?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.191
_refine_diff_density_min         -3.003
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.561
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         10367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.561
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+63.2009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                10337
_reflns_number_total             10367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020269m.cif
_cod_data_source_block           hos179
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076901