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_4511945
_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            'Cl10 Mn9 O16 Sb8'
_chemical_formula_weight         2078.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 102.849(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2744(9)
_cell_length_b                   17.2532(12)
_cell_length_c                   11.0608(10)
_cell_measurement_reflns_used    3242
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3520
_cell_measurement_theta_min      3.4550
_cell_volume                     1539.5(3)
_computing_cell_refinement
;
'Thu May 15 00:28:49 2014'
;
_computing_data_collection
;
'Thu May 15 00:28:49 2014'
;
_computing_data_reduction
;
'Thu May 15 00:28:49 2014'
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.935
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1625
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12893
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.43
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    11.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1862
_exptl_crystal_size_max          0.007
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.862
_refine_diff_density_min         -2.106
_refine_diff_density_rms         0.420
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         12893
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                7698
_reflns_number_total             12893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010374_si_008.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4511945--4511952.cif.'
_cod_original_cell_volume        1539.5(2)
_cod_database_code               4511945