Crystallographic disorder in mixed-valent dioxo-bridged Mn^III,IV^ complexes. [Mn~2~O~2~(bpy)~4~][Ce(NO~3~)~6~].5H~2~O
D. Ramalakshmi; M. V. Rajasekharan; Acta Crystallographica Section B 55 (1999) 186–191; doi:10.1107/S0108768198011586

data_2003075
_publ_section_title
;
 Crystallographic disorder in mixed-valent dioxo-bridged Mn^III,IV^
 complexes. [Mn~2~O~2~(bpy)~4~][Ce(NO~3~)~6~].5H~2~O
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              186
_journal_page_last               191
_journal_paper_doi               10.1107/S0108768198011586
_journal_volume                  55
_journal_year                    1999
_chemical_formula_analytical     'C40 H42 Ce Mn2 N14 025'
_chemical_formula_iupac          '[Mn2 O2 (C10 H8 N2)4][Ce(N O3)6].5(H2 O)'
_chemical_formula_structural     '[Mn2O2(bpy)4][Ce(NO3)6].5H2O'
_chemical_formula_sum            'C40 H42 Ce Mn2 N14 O25'
_chemical_formula_weight         1368.88
_chemical_name_systematic
;
 Tetrakis(2,2'-bipyridine)bis(mu-oxo)dimanganese(3+)
 hexanitratocerate(3-) pentahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.29(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.940(3)
_cell_length_b                   18.060(2)
_cell_length_c                   22.544(11)
_cell_measurement_temperature    132(2)
_cell_volume                     5237(3)
_computing_cell_refinement       'Siemens 1990-4'
_computing_data_collection       'Siemens 1990-4'
_computing_data_reduction        'Siemens 1990-4'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-2\q
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6034
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.327
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            'dark greenish black'
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_meas      1.75
_exptl_crystal_density_method    floatation
_exptl_crystal_description       'rectangular rods'
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.589
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_hydrogen_treatment
;
 Hydrogen atoms are labelled according to the atom to which they are
 attached. All hydrogens except HW1A, HW1B, HW2A, HW2B, HW3A, HW3B,
 HW4A and HW4B were refined using the riding model (the positional
 parameters of the riding atoms have same e.s.ds as the atom on which
 they ride). Bond length constraints were applied to the hydrogens
 of the water molecules. All hydrogens except HW1A, HW1B, HW2A and
 HW2B were assigned fixed U(iso) values (= 1.5 times the U(iso) of
 the atom to which they are attached).
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5645
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.224
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0358
_refine_ls_shift/esd_max
' -0.157 (for y of HW3A, < 0.03 for all non-H atoms)'
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+13.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0947
_refine_ls_wR_factor_obs         0.0783
_reflns_number_observed          4877
_reflns_number_total             6021
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            os0004.cif
_cod_data_source_block           ce2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+13.2986P] 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^)+(0.0342P)^2^+13.2986P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5237.(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2003075