Polynuclear Aggregation of Manganese Dichloride. Syntheses, Properties, and Structures of Polymeric [MnCl2(THF)1.6]\ιnfty, Dimeric [(THF)4Mg(μ-Cl)2MnCl2], and Ionic [Mg(H2O)2(THF)4][Mg(H2O)4(THF)2][MnCl4]2.2THF Compounds
Piotr Sobota; Józef Utko; Lucjan B. Jerzykiewicz; Inorganic Chemistry 37 (1998) 3428–3431; doi:10.1021/ic971513i

data_4322855
_publ_section_title
;
 Polynuclear Aggregation of Manganese Dichloride. Syntheses, Properties,
 and Structures of Polymeric [MnCl2(THF)1.6]\\infty, Dimeric
 [(THF)4Mg(\m-Cl)2MnCl2], and Ionic
 [Mg(H2O)2(THF)4][Mg(H2O)4(THF)2][MnCl4]2.2THF Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3428
_journal_page_last               3431
_journal_paper_doi               10.1021/ic971513i
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C16 H32 Cl5 Mn2.5 O4'
_chemical_formula_weight         603.02
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                74.19(3)
_cell_angle_beta                 76.16(3)
_cell_angle_gamma                77.62(3)
_cell_formula_units_Z            2
_cell_length_a                   9.547(2)
_cell_length_b                   11.191(2)
_cell_length_c                   12.667(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     1248.1(5)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_molecular_graphics    'ORTEP, 1964'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measurement_device       'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta 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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3596
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.807
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       cubic-shape
_exptl_crystal_F_000             615
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_obs          0.0342
_refine_ls_shift/esd_max         0.065
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.2612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1120
_refine_ls_wR_factor_obs         0.0953
_reflns_number_observed          2368
_reflns_number_total             3596
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971513i_1.cif
_cod_data_source_block           compound_1_ic971513L
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0662P)^2^+0.2612P] 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^)+(0.0662P)^2^+0.2612P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C16 H32 Cl5 Mn2.50 O4'
_cod_database_code               4322855