A Synthetic Route toward Layered Materials: Introducing Stereochemically Active Lone-Pairs into Transition Metal Oxohalides
Zimmermann, Iwan; Johnsson, Mats; Crystal Growth & Design 14 (2014) 5252–; doi:10.1021/cg5010374

data_4511947
_publ_section_title
;
 A Synthetic Route toward Layered Materials: Introducing Stereochemically
 Active Lone-Pairs into Transition Metal Oxohalides
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5252
_journal_paper_doi               10.1021/cg5010374
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'Cl8 Fe7 O18 Sb10'
_chemical_formula_weight         2180.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.656(2)
_cell_angle_beta                 65.874(3)
_cell_angle_gamma                63.865(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6600(4)
_cell_length_b                   9.9264(3)
_cell_length_c                   9.8549(3)
_cell_measurement_reflns_used    5976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.5471
_cell_measurement_theta_min      4.2067
_cell_volume                     766.18(5)
_computing_cell_refinement
;
'Thu Aug 09 14:43:14 2012'
;
_computing_data_collection
;
'Thu Aug 09 14:43:14 2012'
;
_computing_data_reduction
;
'Thu Aug 09 14:43:14 2012'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8395
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.63
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    12.613
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Thu Aug 09 14:43:14 2012'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.0489
_exptl_crystal_size_mid          0.0365
_exptl_crystal_size_min          0.0338
_refine_diff_density_max         2.918
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.437
_refine_ls_extinction_coef       0.0048(3)
_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_ref   1.010
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                4648
_reflns_number_total             5321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010374_si_004.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4511945--4511952.cif.'
_cod_database_code               4511947