#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:32:24 +0100 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/70/4317036.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_4317036
loop_
_publ_author_name
'Jiong-Peng Zhao'
'Bo-Wen Hu'
'Francesc Lloret'
'Jun Tao'
'Qian Yang'
'Xiao-Feng Zhang'
'Xian-He Bu'
_publ_section_title
;
 Magnetic Behavior Control in Niccolite Structural Metal Formate
 Frameworks [NH2(CH3)2][FeIIIMII(HCOO)6] (M = Fe, Mn, and Co) by Varying
 the Divalent Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10390
_journal_page_last               10399
_journal_paper_doi               10.1021/ic1014863
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C8 H14 Co Fe N O12'
_chemical_formula_weight         430.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.2486(12)
_cell_length_b                   8.2486(12)
_cell_length_c                   13.790(3)
_cell_measurement_reflns_used    7709
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     812.6(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8184
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0296
_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/[\s^2^(Fo^2^)+(0.0263P)^2^+0.6942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                593
_reflns_number_total             631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1014863_si_002_4.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Co1 Co 0.3333 0.6667 0.2500 0.01530(18) Uani 1 6 d S . .
Fe2 Fe 0.0000 1.0000 0.0000 0.01184(18) Uani 1 6 d S . .
O1 O 0.1178(2) 0.6588(2) 0.16774(12) 0.0309(4) Uani 1 1 d . . .
O2 O -0.0100(2) 0.7929(2) 0.08269(11) 0.0257(3) Uani 1 1 d . . .
C1 C 0.1268(3) 0.7897(3) 0.11996(16) 0.0264(5) Uani 1 1 d . . .
C2 C 0.3333 0.6667 0.844(2) 0.214(12) Uani 1 3 d S . .
N1 N 0.2816(14) 0.563(3) 0.7500 0.20(3) Uani 0.33 2 d SP . .
H1 H 0.244(6) 0.893(6) 0.109(3) 0.071(11) Uiso 1 1 d . . .
H3 H 0.25(2) 0.53(2) 0.708(9) 0.04(4) Uiso 0.33 1 d P . .
H2 H 0.25(3) 0.71(3) 0.892(10) 0.44(9) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0136(2) 0.0136(2) 0.0186(3) 0.000 0.000 0.00681(11)
Fe2 0.0109(2) 0.0109(2) 0.0138(3) 0.000 0.000 0.00543(11)
O1 0.0278(9) 0.0252(8) 0.0395(9) 0.0100(7) -0.0075(7) 0.0129(7)
O2 0.0216(8) 0.0233(8) 0.0329(8) 0.0084(7) -0.0029(7) 0.0118(7)
C1 0.0212(11) 0.0236(11) 0.0336(11) 0.0073(9) -0.0018(9) 0.0105(9)
C2 0.059(4) 0.059(4) 0.53(4) 0.000 0.000 0.0295(18)
N1 0.046(10) 0.015(9) 0.52(9) 0.000 0.10(3) 0.008(4)
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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O1 Co1 O1 89.13(10) 4_665 . ?
O1 Co1 O1 84.65(9) 4_665 3_565 ?
O1 Co1 O1 93.15(7) . 3_565 ?
O1 Co1 O1 93.15(7) 4_665 6_565 ?
O1 Co1 O1 84.65(9) . 6_565 ?
O1 Co1 O1 176.92(9) 3_565 6_565 ?
O1 Co1 O1 176.92(9) 4_665 2_665 ?
O1 Co1 O1 93.15(7) . 2_665 ?
O1 Co1 O1 93.15(7) 3_565 2_665 ?
O1 Co1 O1 89.13(10) 6_565 2_665 ?
O1 Co1 O1 93.15(7) 4_665 5 ?
O1 Co1 O1 176.92(9) . 5 ?
O1 Co1 O1 89.13(10) 3_565 5 ?
O1 Co1 O1 93.15(7) 6_565 5 ?
O1 Co1 O1 84.65(9) 2_665 5 ?
O2 Fe2 O2 180.00(7) 8_455 2_675 ?
O2 Fe2 O2 88.72(7) 8_455 3_465 ?
O2 Fe2 O2 91.28(7) 2_675 3_465 ?
O2 Fe2 O2 91.28(7) 8_455 7_575 ?
O2 Fe2 O2 88.72(7) 2_675 7_575 ?
O2 Fe2 O2 88.72(7) 3_465 7_575 ?
O2 Fe2 O2 91.28(7) 8_455 9_665 ?
O2 Fe2 O2 88.72(7) 2_675 9_665 ?
O2 Fe2 O2 180.0 3_465 9_665 ?
O2 Fe2 O2 91.28(7) 7_575 9_665 ?
O2 Fe2 O2 88.72(7) 8_455 . ?
O2 Fe2 O2 91.28(7) 2_675 . ?
O2 Fe2 O2 91.28(7) 3_465 . ?
O2 Fe2 O2 180.00(9) 7_575 . ?
O2 Fe2 O2 88.72(7) 9_665 . ?
C1 O1 Co1 125.90(15) . . ?
C1 O2 Fe2 126.39(14) . . ?
O1 C1 O2 125.2(2) . . ?
N1 C2 N1 50.7(16) 3_565 . ?
N1 C2 N1 50.7(16) 3_565 2_665 ?
N1 C2 N1 50.7(16) . 2_665 ?
N1 N1 N1 60.0 2_665 3_565 ?
N1 N1 C2 64.7(8) 2_665 . ?
N1 N1 C2 64.7(8) 3_565 . ?
N1 N1 C2 64.7(8) 2_665 4_666 ?
N1 N1 C2 64.7(8) 3_565 4_666 ?
C2 N1 C2 120.7(19) . 4_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.0825(15) 4_665 ?
Co1 O1 2.0825(15) . ?
Co1 O1 2.0825(15) 3_565 ?
Co1 O1 2.0825(15) 6_565 ?
Co1 O1 2.0825(15) 2_665 ?
Co1 O1 2.0825(15) 5 ?
Fe2 O2 2.0208(15) 8_455 ?
Fe2 O2 2.0208(15) 2_675 ?
Fe2 O2 2.0208(15) 3_465 ?
Fe2 O2 2.0208(15) 7_575 ?
Fe2 O2 2.0208(15) 9_665 ?
Fe2 O2 2.0208(15) . ?
O1 C1 1.235(3) . ?
O2 C1 1.252(3) . ?
C2 N1 1.50(3) 3_565 ?
C2 N1 1.50(3) . ?
C2 N1 1.50(3) 2_665 ?
N1 N1 1.28(3) 2_665 ?
N1 N1 1.28(3) 3_565 ?
N1 C2 1.50(3) 4_666 ?
