#------------------------------------------------------------------------------
#$Date: 2015-08-08 05:25:30 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153198 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/54/7035406.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_7035406
loop_
_publ_author_name
'Ciupa, Aneta'
'Mączka, Mirosław'
'Gągor, Anna'
'Pikul, Adam'
'Ptak, Maciej'
_publ_section_title
;
 Synthesis and characterization of novel niccolites
 [(CH3)2NH2][Fe(III)M(II)(HCOO)6] (M(II) = Zn, Ni, Cu).
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13234
_journal_page_last               13241
_journal_paper_doi               10.1039/c5dt01608h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C8 H14 Fe N Ni O12'
_chemical_formula_weight         430.76
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.1856(7)
_cell_length_b                   8.1856(7)
_cell_length_c                   13.6517(17)
_cell_measurement_reflns_used    1320
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5969
_cell_measurement_theta_min      2.8676
_cell_volume                     792.17(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.4350
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5333
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.593
_diffrn_reflns_theta_max         25.593
_diffrn_reflns_theta_min         2.873
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       needle
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         507
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0055P)²+2.2800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                391
_reflns_number_total             507
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01608h2.cif
_cod_data_source_block           nife
_cod_depositor_comments
'Adding full bibliography for 7035405--7035406.cif.'
_cod_original_cell_volume        792.17(17)
_cod_database_code               7035406
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.3333 0.6667 0.2500 0.0147(4) Uani 0.493(7) 6 d S T P
Ni1 Ni 0.3333 0.6667 0.2500 0.0147(4) Uani 0.507(7) 6 d S T P
Fe2 Fe 0.0000 1.0000 0.0000 0.0138(4) Uani 0.509(7) 6 d S T P
Ni2 Ni 0.0000 1.0000 0.0000 0.0138(4) Uani 0.490(7) 6 d S T P
O1 O 0.1224(4) 0.6594(4) 0.1686(2) 0.0277(7) Uani 1 1 d . . .
O2 O -0.0094(4) 0.7911(4) 0.0833(2) 0.0251(7) Uani 1 1 d . . .
C1 C 0.1287(6) 0.7897(6) 0.1205(3) 0.0272(10) Uani 1 1 d . . .
H1 H 0.2465 0.8961 0.1113 0.033 Uiso 1 1 calc R U .
C2 C 0.3333 0.6667 0.8752(15) 0.094(7) Uani 0.5 3 d DS TU P
H2A H 0.4599 0.7716 0.8739 0.140 Uiso 0.1667 1 calc R U P
H2B H 0.3217 0.5817 0.9267 0.140 Uiso 0.1667 1 calc R U P
H2C H 0.2468 0.7116 0.8866 0.140 Uiso 0.1667 1 calc R U P
C21 C 0.3333 0.6667 0.690(2) 0.094(7) Uani 0.5 3 d DS TU P
H21A H 0.4632 0.7124 0.6740 0.140 Uiso 0.1667 1 calc R U P
H21B H 0.3113 0.7711 0.6951 0.140 Uiso 0.1667 1 calc R U P
H21C H 0.2540 0.5817 0.6401 0.140 Uiso 0.1667 1 calc R U P
N1 N 0.291(5) 0.569(4) 0.7824(14) 0.051(9) Uiso 0.1667 1 d D . P
H1A H 0.3543 0.4950 0.7790 0.061 Uiso 0.1667 1 d . U P
H1B H 0.1671 0.4706 0.7790 0.061 Uiso 0.1667 1 d . U P
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
N N 0.0061 0.0033 '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
O1 Fe1 O1 92.87(12) 4_665 6_565
O1 Fe1 O1 85.06(17) 4_665 3_565
O1 Fe1 O1 177.09(18) 6_565 3_565
O1 Fe1 O1 177.09(18) 4_665 2_665
O1 Fe1 O1 89.27(18) 6_565 2_665
O1 Fe1 O1 92.87(12) 3_565 2_665
O1 Fe1 O1 92.87(12) 4_665 5
O1 Fe1 O1 92.87(12) 6_565 5
O1 Fe1 O1 89.27(18) 3_565 5
O1 Fe1 O1 85.06(17) 2_665 5
O1 Fe1 O1 89.27(18) 4_665 .
O1 Fe1 O1 85.06(17) 6_565 .
O1 Fe1 O1 92.87(12) 3_565 .
O1 Fe1 O1 92.87(12) 2_665 .
O1 Fe1 O1 177.09(18) 5 .
O2 Fe2 O2 180.00(14) 8_455 2_675
O2 Fe2 O2 91.47(12) 8_455 9_665
O2 Fe2 O2 88.53(12) 2_675 9_665
O2 Fe2 O2 91.47(12) 8_455 7_575
O2 Fe2 O2 88.53(12) 2_675 7_575
O2 Fe2 O2 91.47(12) 9_665 7_575
O2 Fe2 O2 88.53(12) 8_455 3_465
O2 Fe2 O2 91.47(12) 2_675 3_465
O2 Fe2 O2 180.0 9_665 3_465
O2 Fe2 O2 88.53(12) 7_575 3_465
O2 Fe2 O2 88.52(12) 8_455 .
O2 Fe2 O2 91.48(12) 2_675 .
O2 Fe2 O2 88.52(12) 9_665 .
O2 Fe2 O2 180.0 7_575 .
O2 Fe2 O2 91.48(12) 3_465 .
C1 O1 Fe1 126.9(3) . .
C1 O2 Fe2 125.9(3) . .
O1 C1 O2 125.5(4) . .
C21 N1 C2 122(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.029(3) 4_665
Fe1 O1 2.029(3) 6_565
Fe1 O1 2.029(3) 3_565
Fe1 O1 2.029(3) 2_665
Fe1 O1 2.029(3) 5
Fe1 O1 2.029(3) .
Fe2 O2 2.023(3) 8_455
Fe2 O2 2.023(3) 2_675
Fe2 O2 2.023(3) 9_665
Fe2 O2 2.023(3) 7_575
Fe2 O2 2.023(3) 3_465
Fe2 O2 2.023(3) .
O1 C1 1.231(5) .
O2 C1 1.244(5) .
C2 N1 1.444(10) .
C21 N1 1.436(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.98 2.41 3.25(3) 143.7 11_666
N1 H1A O1 0.98 2.45 3.23(3) 136.1 8_556
N1 H1B O1 0.93 2.18 3.01(3) 148.9 7_566
C2 H2C O2 0.96 2.53 3.385(5) 147.8 9_666
