Structural characterization of methanol substituted lanthanum halides
Timothy J. Boyle; Leigh Anna M. Ottley; Todd M. Alam; Mark A. Rodriguez; Pin Yang; Sarah K. Mcintyre; Polyhedron 29 (2010) 1784–1795; doi:10.1016/j.poly.2010.02.027

data_1512926
_publ_section_title
;
 Structural characterization of methanol substituted lanthanum halides
;
_journal_issue                   7
_journal_name_full               Polyhedron
_journal_page_first              1784
_journal_page_last               1795
_journal_paper_doi               10.1016/j.poly.2010.02.027
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety
'C5.75 H20 Br2.25 La O5.75, C4.25 H16 Br3.75 La O4.25'
_chemical_formula_sum            'C5 H20 Br3 La O5'
_chemical_formula_weight         537.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 106.532(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1803(16)
_cell_length_b                   14.794(2)
_cell_length_c                   10.6387(17)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      1.38
_cell_volume                     1536.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10742
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    10.581
_exptl_absorpt_correction_T_max  0.4848
_exptl_absorpt_correction_T_min  0.3600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fiber
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+1.0542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                5051
_reflns_number_total             5269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2010-1784.cif
_cod_data_source_block           7sp212p
_cod_depositor_comments
;

  The following markup was applied to this entry, as discussed with
  the corresponding author T. J. Boyle:

  a) disordered fragments (Br3, C7, O7) and (Br7, C3, O3) were
  assigned to two distinct disorder groups 1 and 2, as is described in
  the original paper;

  b) _atom_site_attached_hydrogens were added and hydrogen count 3 was
  set for C3 and C7, and hydrogen count 1 for O3 and O7, to agree with
  the chemical nature of the moyety and as described in the original
  paper text.

  c) The _chemical_formula_sum was changed to 'C10 H36 Br6 La2 O10';
  this value can be obtained from the coordinates *without* taking
  _atom_site_attached_hydrogens into account. This formula was chosen
  because it i) corresponds to the _chemical_formula_moiety provided
  by the authors and ii) matches the formula of compound 4 in the
  Table 2 of the original paper.

  Saulius Gra\<zulis
  2013-12-06
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_cod_original_sg_symbol_H-M      Pc
_cod_original_formula_sum        'C10 H38 Br6 La2 O10'
_cod_database_code               1512926