Synthesis and Characterization of a Tetrapodal NO4(4-) Ligand and Its Transition Metal Complexes.
Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R.; Chang, Christopher J.; Long, Jeffrey R.; Inorganic chemistry 55 (2016) 7527–7534; doi:10.1021/acs.inorgchem.6b00908

data_4348036
_publ_section_title
;
 Synthesis and Characterization of a Tetrapodal NO4(4-) Ligand and Its
 Transition Metal Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7527
_journal_page_last               7534
_journal_paper_doi               10.1021/acs.inorgchem.6b00908
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C13 H15 Fe K2 N O11'
_chemical_formula_sum            'C13 H15 Fe K2 N O11'
_chemical_formula_weight         495.30
_chemical_name_common            jaa24
_chemical_name_systematic        'K2[(C13H9NO8)Fe(H2O)] 2(H2O)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                81.500(2)
_cell_angle_beta                 88.018(2)
_cell_angle_gamma                86.820(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5937(4)
_cell_length_b                   10.3520(4)
_cell_length_c                   10.9128(5)
_cell_measurement_reflns_used    5815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.94
_cell_volume                     846.82(7)
_computing_cell_refinement       'Buker APEX2 v. 2011.4'
_computing_data_collection       'Buker APEX2 v. 2011.4'
_computing_data_reduction        'Buker APEX2 v. 2011.4'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14312
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.888
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0967 before and 0.0464 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1126 before and 0.0495 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 14312 reflections, Rint = 0.0481
 (8385 with I > 3sig(I), Rint = 0.0420)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         9131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.3685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7942
_reflns_number_total             9131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jaa24.cif
_cod_data_source_block           shelx
_cod_database_code               4348036
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.883
_shelx_res_checksum              82829
_shelx_hkl_checksum              4343