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_4348042
_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 H13 K2 Mn N O10'
_chemical_formula_sum            'C13 H13 K2 Mn N O10'
_chemical_formula_weight         476.38
_chemical_name_common            jaa20_0m
_chemical_name_systematic        'K2[(C13H9NO8)Mn(H2O)] H2O'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3220(2)
_cell_length_b                   10.9900(3)
_cell_length_c                   20.2140(6)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.96
_cell_volume                     1626.60(8)
_computing_cell_refinement       'Bruker APEX2 v. 2011.4'
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_computing_molecular_graphics    DIAMOND
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_computing_structure_solution    Sir-2004
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0414P)^2^+2.1602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1353
_reflns_number_total             1487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jaa20_0m.cif
_cod_data_source_block           shelx
_cod_database_code               4348042
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              82243
_shelx_hkl_checksum              79250