Synthesis and Structure of the First Tetranuclear Organolanthanide Cluster Containing aμ4-Imido Group
Xie, Zuowei; Wang, Shaowu; Yang, Qingchuan; Mak, Thomas C. W.; Organometallics 18 (1999) 1578–; doi:10.1021/om981002j

data_4077751
_publ_section_title
;
 Synthesis and Structure of the First Tetranuclear Organolanthanide
 Cluster Containing a\m4-Imido Group
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1578
_journal_paper_doi               10.1021/om981002j
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C56 H77 Cl2 Gd4 N5 O3 Si4'
_chemical_formula_weight         1680.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6250(15)
_cell_length_b                   19.2260(15)
_cell_length_c                   15.1250(10)
_cell_measurement_reflns_used    291
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52
_cell_measurement_theta_min      4
_cell_volume                     6288.4(8)
_computing_cell_refinement       'BIOTEX RIGAKU'
_computing_data_collection       'RAXIS RIGAKU'
_computing_molecular_graphics    'SEIMENS SHELTXL'
_computing_publication_material  'SEIMENS SHELTXL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       IP-RIGAKU
_diffrn_measurement_method       IP
_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  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10116
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    4.369
_exptl_absorpt_correction_T_max  1.240
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            COLOLESS
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_meas      ?
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.250
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_coef       0.00082(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_obs          0.0631
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+3.2918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1597
_refine_ls_wR_factor_obs         0.1583
_reflns_number_observed          2959
_reflns_number_total             3018
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om981002j.cif
_cod_data_source_block           cluster_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'ORTHORHOMBIC' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+3.2918P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+3.2918P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Aba2
_cod_database_code               4077751