#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:02:42 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180285 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/71/7117109.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_7117109
loop_
_publ_author_name
'Jiong-Peng Zhao'
'Song-De Han'
'Xue Jiang'
'Sui-Jun Liu'
'Ran Zhao'
'Ze Chang'
'Xian-He Bu'
_publ_section_title
;
 A heterometallic strategy to achieve a large magnetocaloric effect in
 polymeric 3d complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8288
_journal_paper_doi               10.1039/C5cc00915D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C7 H12 Cr Mn N O12'
_chemical_formula_weight         409.12
_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
_audit_update_record
;
2015-03-06 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.2708(12)
_cell_length_b                   8.2708(12)
_cell_length_c                   14.088(3)
_cell_measurement_reflns_used    7695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     834.6(2)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC'2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω 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  0.0418
_diffrn_reflns_av_unetI/netI     0.0157
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8248
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         644
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0442
_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)+(0.0617P)²+1.5954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                609
_reflns_number_total             644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00915d2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               7117109
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
Mn1 Mn 0.6667 0.3333 0.2500 0.0172(3) Uani 1 6 d S . .
Cr1 Cr 0.0000 0.0000 0.0000 0.0141(3) Uani 1 6 d S . .
O2 O 0.4485(4) 0.3378(4) 0.16533(19) 0.0366(7) Uani 1 1 d . . .
O1 O 0.1902(3) 0.2040(3) 0.07992(17) 0.0254(5) Uani 1 1 d . . .
C1 C 0.3320(5) 0.2099(5) 0.1160(3) 0.0305(8) Uani 1 1 d . . .
H1A H 0.3502 0.1094 0.1046 0.037 Uiso 1 1 calc R . .
N1 N 0.2738(15) 0.548(3) 0.2500 0.068(5) Uani 0.33 2 d SPDU . .
H3B H 0.3143 0.6300 0.2988 0.082 Uiso 0.17 1 d PR . .
H3A H 0.3264 0.4685 0.2500 0.082 Uiso 0.33 1 d PR . .
C2 C 0.3333 0.6667 0.136(3) 0.15(2) Uani 0.50 3 d SPD . .
H2 H 0.3386 0.7491 0.0982 0.184 Uiso 0.50 1 d PR . .
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
Mn1 0.0156(4) 0.0156(4) 0.0204(6) 0.000 0.000 0.0078(2)
Cr1 0.0132(4) 0.0132(4) 0.0160(6) 0.000 0.000 0.0066(2)
O2 0.0312(14) 0.0333(14) 0.0462(15) -0.0146(12) -0.0204(12) 0.0167(12)
O1 0.0220(12) 0.0231(12) 0.0317(12) -0.0085(10) -0.0096(10) 0.0118(10)
C1 0.0254(16) 0.0272(17) 0.0406(19) -0.0083(15) -0.0120(15) 0.0143(14)
N1 0.049(6) 0.063(8) 0.098(9) 0.000 0.015(7) 0.032(4)
C2 0.083(13) 0.083(13) 0.30(7) 0.000 0.000 0.041(7)
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
O2 Mn1 O2 88.35(16) 5_655 2_655
O2 Mn1 O2 85.91(14) 5_655 3_665
O2 Mn1 O2 92.88(11) 2_655 3_665
O2 Mn1 O2 92.88(11) 5_655 6
O2 Mn1 O2 85.91(14) 2_655 6
O2 Mn1 O2 178.32(14) 3_665 6
O2 Mn1 O2 92.88(11) 5_655 4_665
O2 Mn1 O2 178.32(14) 2_655 4_665
O2 Mn1 O2 88.35(16) 3_665 4_665
O2 Mn1 O2 92.88(11) 6 4_665
O2 Mn1 O2 178.32(14) 5_655 .
O2 Mn1 O2 92.88(11) 2_655 .
O2 Mn1 O2 92.88(11) 3_665 .
O2 Mn1 O2 88.35(16) 6 .
O2 Mn1 O2 85.91(14) 4_665 .
O1 Cr1 O1 180.00(17) 7 .
O1 Cr1 O1 89.04(10) 7 2
O1 Cr1 O1 90.96(10) . 2
O1 Cr1 O1 90.96(10) 7 9
O1 Cr1 O1 89.04(10) . 9
O1 Cr1 O1 89.04(10) 2 9
O1 Cr1 O1 89.04(10) 7 3
O1 Cr1 O1 90.96(10) . 3
O1 Cr1 O1 90.96(10) 2 3
O1 Cr1 O1 180.00(16) 9 3
O1 Cr1 O1 90.96(10) 7 8
O1 Cr1 O1 89.04(10) . 8
O1 Cr1 O1 180.00(14) 2 8
O1 Cr1 O1 90.96(10) 9 8
O1 Cr1 O1 89.04(10) 3 8
C1 O2 Mn1 126.5(2) . .
C1 O1 Cr1 126.2(2) . .
O2 C1 O1 125.3(3) . .
O2 C1 H1A 117.4 . .
O1 C1 H1A 117.4 . .
N1 N1 N1 60.0 2_665 3_565
N1 N1 C2 66.1(8) 2_665 4_665
N1 N1 C2 66.1(8) 3_565 4_665
N1 N1 C2 66.1(8) 2_665 .
N1 N1 C2 66.1(8) 3_565 .
C2 N1 C2 124(2) 4_665 .
N1 N1 H3B 55.9 2_665 .
N1 N1 H3B 55.5 3_565 .
C2 N1 H3B 12.7 4_665 .
C2 N1 H3B 111.4 . .
N1 N1 H3A 96.6 2_665 .
N1 N1 H3A 156.6 3_565 .
C2 N1 H3A 106.2 4_665 .
C2 N1 H3A 106.2 . .
H3B N1 H3A 113.2 . .
N1 C2 N1 47.9(17) 3_565 2_665
N1 C2 N1 47.9(17) 3_565 .
N1 C2 N1 47.9(17) 2_665 .
N1 C2 H2 104.3 3_565 .
N1 C2 H2 122.1 2_665 .
N1 C2 H2 151.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.179(2) 5_655
Mn1 O2 2.179(2) 2_655
Mn1 O2 2.179(2) 3_665
Mn1 O2 2.179(2) 6
Mn1 O2 2.179(2) 4_665
Mn1 O2 2.179(2) .
Cr1 O1 1.983(2) 7
Cr1 O1 1.983(2) .
Cr1 O1 1.983(2) 2
Cr1 O1 1.983(2) 9
Cr1 O1 1.983(2) 3
Cr1 O1 1.983(2) 8
O2 C1 1.229(4) .
O1 C1 1.257(4) .
C1 H1A 0.9300 .
N1 N1 1.48(4) 2_665
N1 N1 1.48(4) 3_565
N1 C2 1.82(4) 4_665
N1 C2 1.82(4) .
N1 H3B 0.9062 .
N1 H3A 0.9499 .
C2 N1 1.82(4) 3_565
C2 N1 1.82(4) 2_665
C2 H2 0.8474 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O2 Mn1 O2 C1 159.7(3) 5_655 . . .
O2 Mn1 O2 C1 22.6(3) 2_655 . . .
O2 Mn1 O2 C1 115.7(3) 3_665 . . .
O2 Mn1 O2 C1 -63.2(3) 6 . . .
O2 Mn1 O2 C1 -156.2(4) 4_665 . . .
O1 Cr1 O1 C1 -21.8(3) 7 . . .
O1 Cr1 O1 C1 129.5(3) 2 . . .
O1 Cr1 O1 C1 -141.5(3) 9 . . .
O1 Cr1 O1 C1 38.5(3) 3 . . .
O1 Cr1 O1 C1 -50.5(3) 8 . . .
Mn1 O2 C1 O1 168.1(3) . . . .
Cr1 O1 C1 O2 179.9(3) . . . .
N1 N1 C2 N1 -66.3(5) 2_665 . . 3_565
C2 N1 C2 N1 -33.2(2) 4_665 . . 3_565
N1 N1 C2 N1 66.3(5) 3_565 . . 2_665
C2 N1 C2 N1 33.2(2) 4_665 . . 2_665
