#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000201.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000201
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm021212t
_journal_year                    2002
_chemical_formula_sum            'C14 H18 Mn N2 O9'
_chemical_formula_weight         413.24
_chemical_name_systematic
;
poly[diaqua-(mu2-squarato-O,O')-(mu2-4,4`-bipyridine-N,N')-manganese(II)] trihyd
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.536(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7156(12)
_cell_length_b                   11.5444(8)
_cell_length_c                   8.1738(5)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     1766.0(2)
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'STOE Imaging Plate Diffraction system'
_diffrn_measurement_method       'Phi 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14775
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0342
_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/[σ²(Fo²)+(0.0445P)²+0.8945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                3254
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4000201
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 1.0000 0.5000 0.01156(10) Uani 1 2 d S . .
O1 O 0.45493(5) 0.96761(9) 0.74207(13) 0.0160(2) Uani 1 1 d . . .
C1 C 0.48024(7) 0.98554(11) 0.88266(18) 0.0130(3) Uani 1 1 d . . .
C2 C 0.53285(7) 1.06545(11) 0.95589(17) 0.0131(3) Uani 1 1 d . . .
O2 O 0.57158(6) 1.14562(9) 0.90344(13) 0.0165(2) Uani 1 1 d . . .
O5 O 0.55004(6) 1.15872(9) 0.58138(15) 0.0193(2) Uani 1 1 d . . .
H1 H 0.5660(15) 1.219(2) 0.529(3) 0.042(7) Uiso 1 1 d . . .
H2 H 0.5626(13) 1.165(2) 0.682(4) 0.035(6) Uiso 1 1 d . . .
Mn2 Mn 1.0000 0.5000 1.0000 0.01162(10) Uani 1 2 d S . .
O3 O 1.03731(6) 0.54620(9) 0.75958(13) 0.0178(2) Uani 1 1 d . . .
C3 C 1.01624(8) 0.51998(12) 0.61806(18) 0.0140(3) Uani 1 1 d . . .
C4 C 1.03109(7) 0.56741(12) 0.45600(17) 0.0141(3) Uani 1 1 d . . .
O4 O 1.06808(6) 0.65017(9) 0.40434(13) 0.0182(2) Uani 1 1 d . . .
O6 O 1.04762(6) 0.65836(9) 1.08483(14) 0.0182(2) Uani 1 1 d . . .
H3 H 1.0651(13) 0.718(2) 1.032(3) 0.029(5) Uiso 1 1 d . . .
H4 H 1.0594(14) 0.671(2) 1.184(4) 0.036(6) Uiso 1 1 d . . .
N1 N 0.59884(7) 0.90567(11) 0.59970(16) 0.0163(2) Uani 1 1 d . . .
C11 C 0.71565(7) 0.78515(12) 0.73507(18) 0.0163(3) Uani 1 1 d . . .
C12 C 0.64898(8) 0.73238(13) 0.7168(2) 0.0207(3) Uani 1 1 d . . .
H12 H 0.6422 0.6542 0.7496 0.025 Uiso 1 1 calc R . .
C13 C 0.59274(8) 0.79516(13) 0.6504(2) 0.0200(3) Uani 1 1 d . . .
H13 H 0.5475 0.7584 0.6400 0.024 Uiso 1 1 calc R . .
C14 C 0.66260(8) 0.95658(12) 0.6189(2) 0.0191(3) Uani 1 1 d . . .
H14 H 0.6678 1.0348 0.5849 0.023 Uiso 1 1 calc R . .
C15 C 0.72177(8) 0.90032(13) 0.6862(2) 0.0194(3) Uani 1 1 d . . .
H15 H 0.7659 0.9401 0.6988 0.023 Uiso 1 1 calc R . .
N2 N 0.89557(6) 0.59699(11) 0.92993(16) 0.0176(3) Uani 1 1 d . . .
C21 C 0.77776(7) 0.72087(12) 0.80327(18) 0.0161(3) Uani 1 1 d . . .
C22 C 0.83283(8) 0.77667(13) 0.8883(2) 0.0198(3) Uani 1 1 d . . .
H22 H 0.8314 0.8581 0.9044 0.024 Uiso 1 1 calc R . .
C23 C 0.88961(8) 0.71247(13) 0.9491(2) 0.0205(3) Uani 1 1 d . . .
H23 H 0.9264 0.7520 1.0076 0.025 Uiso 1 1 calc R . .
C24 C 0.84224(8) 0.54346(13) 0.8492(2) 0.0195(3) Uani 1 1 d . . .
H24 H 0.8450 0.4619 0.8357 0.023 Uiso 1 1 calc R . .
C25 C 0.78322(8) 0.60105(13) 0.7845(2) 0.0195(3) Uani 1 1 d . . .
H25 H 0.7469 0.5592 0.7279 0.023 Uiso 1 1 calc R . .
O7 O 0.68427(7) 0.36861(12) 0.73740(18) 0.0296(3) Uani 1 1 d . . .
H5 H 0.6427(17) 0.381(3) 0.743(4) 0.047(8) Uiso 1 1 d . . .
H6 H 0.706(3) 0.332(4) 0.815(6) 0.117(17) Uiso 1 1 d . . .
O8 O 0.75185(7) 0.25064(13) 0.48861(16) 0.0292(3) Uani 1 1 d . . .
H7 H 0.783(4) 0.285(6) 0.409(8) 0.17(2) Uiso 1 1 d . . .
H8 H 0.723(3) 0.291(5) 0.580(7) 0.136(19) Uiso 1 1 d . . .
O9 O 0.82028(7) 0.13145(13) 0.74035(18) 0.0302(3) Uani 1 1 d . . .
H9 H 0.8639(17) 0.120(2) 0.740(3) 0.045(7) Uiso 1 1 d . . .
H10 H 0.803(3) 0.168(5) 0.676(6) 0.119(18) Uiso 1 1 d . . .
