#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:46:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179935 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/30/7023090.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_7023090
loop_
_publ_author_name
'Alborés, Pablo'
'Rentschler, Eva'
_publ_section_title
;
 Expanding the 2,2'-bipyrimidine bridged 1D homonuclear coordination
 polymers family: [M(II)(bpym)Cl2] (M = Fe, Co) magnetic and structural
 characterization.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9621
_journal_page_last               9627
_journal_paper_doi               10.1039/c3dt50691f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C21 H12 Cl4 Fe2 N10 O'
_chemical_formula_weight         673.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.978(4)
_cell_length_b                   16.464(5)
_cell_length_c                   29.114(9)
_cell_measurement_temperature    173(2)
_cell_volume                     5741(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15768
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  1.1165
_exptl_absorpt_correction_T_min  0.5438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1739
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0584
_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/[σ²(Fo²)+(0.0562P)²+65.3994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                1289
_reflns_number_total             1739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50691f.txt
_cod_data_source_block           1
_cod_original_cell_volume        5741(5)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7023090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
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
Fe1 Fe 0.1250 0.1250 0.30251(3) 0.0264(3) Uani 1 2 d S . .
Cl2 Cl 0.19268(10) 0.22199(7) 0.35620(4) 0.0375(3) Uani 1 1 d . . .
N1 N -0.0448(3) 0.1738(2) 0.29042(12) 0.0266(8) Uani 1 1 d . . .
N2 N 0.1067(3) 0.0329(2) 0.24594(12) 0.0281(8) Uani 1 1 d . . .
C5 C -0.0515(3) 0.2384(2) 0.26207(13) 0.0228(8) Uani 1 1 d . . .
C6 C -0.1392(4) 0.1538(3) 0.31255(15) 0.0326(10) Uani 1 1 d . . .
H6 H -0.1385 0.1084 0.3327 0.039 Uiso 1 1 calc R . .
C7 C -0.2372(4) 0.1969(3) 0.30712(16) 0.0349(11) Uani 1 1 d . . .
H7 H -0.3031 0.1825 0.3234 0.042 Uiso 1 1 calc R . .
C9 C 0.0147(4) 0.0120(3) 0.22313(16) 0.0331(10) Uani 1 1 d . . .
H9 H -0.0516 0.0427 0.2277 0.040 Uiso 1 1 calc R . .
C3S C 0.3509(15) 0.3575(10) 0.4394(7) 0.068(5) Uani 0.50 1 d P . .
N1S N 0.2667(10) 0.2925(8) 0.4767(4) 0.073(3) Uani 0.50 1 d P . .
C2S C 0.3239(14) 0.3366(10) 0.4600(6) 0.048(3) Uani 0.50 1 d P . .
C1S C -0.077(3) 0.3750 0.3750 0.148(16) Uani 0.50 2 d SPD . .
O2S O 0.038(4) 0.3750 0.3750 0.135(19) Uani 0.1088(19) 2 d SPD A 1
O3S O -0.1250 0.3750 0.332(2) 0.135(19) Uani 0.001(18) 2 d SPD . 2
O4S O -0.001(4) 0.3553(13) 0.3410(8) 0.135(19) Uani 0.195(9) 1 d PD A 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 N1 161.72(18) 2 .
N1 Fe1 N2 92.24(13) 2 2
N1 Fe1 N2 74.24(13) . 2
N1 Fe1 N2 74.24(13) 2 .
N1 Fe1 N2 92.24(13) . .
N2 Fe1 N2 85.86(19) 2 .
N1 Fe1 Cl2 92.01(10) 2 .
N1 Fe1 Cl2 100.01(10) . .
N2 Fe1 Cl2 89.74(10) 2 .
N2 Fe1 Cl2 165.36(9) . .
N1 Fe1 Cl2 100.01(10) 2 2
N1 Fe1 Cl2 92.01(10) . 2
N2 Fe1 Cl2 165.36(9) 2 2
N2 Fe1 Cl2 89.74(10) . 2
Cl2 Fe1 Cl2 97.77(7) . 2
C6 N1 C5 116.0(4) . .
C6 N1 Fe1 127.4(3) . .
C5 N1 Fe1 116.0(3) . .
C9 N2 C5 116.8(4) . 26
C9 N2 Fe1 128.3(3) . .
C5 N2 Fe1 114.5(3) 26 .
N2 C5 N1 125.8(4) 22 .
N2 C5 C5 117.6(4) 22 21
N1 C5 C5 116.6(4) . 21
N1 C6 C7 122.4(4) . .
C6 C7 C9 117.1(4) . 22
N2 C9 C7 122.0(4) . 26
C2S C3S C3S 128(2) . 14
C2S C3S C2S 103(3) . 14
C3S C3S C2S 24.9(10) 14 14
C2S C3S N1S 15(2) . .
C3S C3S N1S 143.6(7) 14 .
C2S C3S N1S 118.7(16) 14 .
C2S N1S C3S 10.4(13) . .
C3S C2S N1S 154(3) . .
C3S C2S C3S 26.8(18) . 14
N1S C2S C3S 178.5(19) . 14
C3S C2S C2S 52(2) . 14
N1S C2S C2S 154.0(11) . 14
C3S C2S C2S 24.9(10) 14 14
C1S C1S O2S 180.000(12) 14_455 .
C1S C1S O3S 65(2) 14_455 .
O2S C1S O3S 115(2) . .
C1S C1S O3S 65(2) 14_455 7
O2S C1S O3S 115(2) . 7
O3S C1S O3S 130(4) . 7
C1S C1S O4S 131(2) 14_455 7
O2S C1S O4S 49(2) . 7
O3S C1S O4S 158(3) . 7
O3S C1S O4S 68.0(17) 7 7
C1S C1S O4S 131(2) 14_455 .
O2S C1S O4S 49(2) . .
O3S C1S O4S 68.0(17) . .
O3S C1S O4S 158(3) 7 .
O4S C1S O4S 98(4) 7 .
C1S O3S C1S 50(4) . 14_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.215(4) 2
Fe1 N1 2.215(4) .
Fe1 N2 2.249(4) 2
Fe1 N2 2.249(4) .
Fe1 Cl2 2.3771(13) .
Fe1 Cl2 2.3771(13) 2
N1 C6 1.342(6) .
N1 C5 1.349(5) .
N2 C9 1.332(6) .
N2 C5 1.341(5) 26
C5 N2 1.341(5) 22
C5 C5 1.469(8) 21
C6 C7 1.380(6) .
C7 C9 1.388(7) 22
C9 C7 1.388(7) 26
C3S C2S 0.761(18) .
C3S C3S 0.82(3) 14
C3S C2S 1.42(2) 14
C3S N1S 1.826(19) .
N1S C2S 1.110(18) .
C2S C3S 1.42(2) 14
C2S C2S 1.76(3) 14
C1S C1S 1.16(7) 14_455
C1S O2S 1.37(4) .
C1S O3S 1.38(5) .
C1S O3S 1.38(5) 7
C1S O4S 1.38(4) 7
C1S O4S 1.38(4) .
O3S C1S 1.38(5) 14_455
