Synthesis and characterization of novel niccolites [(CH3)2NH2][Fe(III)M(II)(HCOO)6] (M(II) = Zn, Ni, Cu).
Ciupa, Aneta; Mączka, Mirosław; Gągor, Anna; Pikul, Adam; Ptak, Maciej; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13234–13241; doi:10.1039/c5dt01608h

data_7035406
_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/[\s^2^(Fo^2^)+(0.0055P)^2^+2.2800P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_res_checksum              46426