Accessing sodium ferrate complexes containing neutral and anionic N-heterocyclic carbene ligands: structural, synthetic, and magnetic insights.
Maddock, Lewis C. H.; Cadenbach, Thomas; Kennedy, Alan R.; Borilovic, Ivana; Aromí, Guillem; Hevia, Eva; Inorganic chemistry 54 (2015) 9201–9210; doi:10.1021/acs.inorgchem.5b01638

data_4346530
_publ_section_title
;
 Accessing sodium ferrate complexes containing neutral and anionic
 N-heterocyclic carbene ligands: structural, synthetic, and magnetic
 insights.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9201
_journal_page_last               9210
_journal_paper_doi               10.1021/acs.inorgchem.5b01638
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C51 H95 Fe N4 Na O3 Si4'
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_space_group_name_Hall           'P 2ac 2ab'
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2296(3)
_cell_length_b                   18.0203(4)
_cell_length_c                   21.9241(6)
_cell_measurement_reflns_used    11587
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1396
_cell_measurement_theta_min      3.0430
_cell_volume                     6016.9(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25202
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         30.207
_diffrn_reflns_theta_min         3.049
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       plates
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 3048 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.019(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         13981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.613
_reflns_Friedel_fraction_full    0.769
_reflns_Friedel_fraction_max     0.650
_reflns_number_gt                10724
_reflns_number_total             13981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01638_si_002.cif
_cod_data_source_block           lewis_20
_cod_database_code               4346530
_shelxl_version_number           2013-3
_shelx_res_checksum              27709
_shelx_hkl_checksum              87380