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_4511950
_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            'Br4 Fe3 O4 Sb2'
_chemical_formula_weight         794.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.30990(10)
_cell_length_b                   12.3959(3)
_cell_length_c                   14.5287(3)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.1031
_cell_measurement_theta_min      3.2217
_cell_volume                     1136.39(4)
_computing_cell_refinement
;
'Fri Aug 10 13:17:09 2012'
;
_computing_data_collection
;
'Fri Aug 10 13:17:09 2012'
;
_computing_data_reduction
;
'Fri Aug 10 13:17:09 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 0.998
_diffrn_measured_fraction_theta_max 0.955
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5118
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.05
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    22.471
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.120
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Fri Aug 10 13:17:09 2012'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.1301
_exptl_crystal_size_mid          0.0494
_exptl_crystal_size_min          0.0282
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                812
_reflns_number_total             1030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010374_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4511945--4511952.cif.'
_cod_database_code               4511950