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_4348032
_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         'C11 H15 Cl Cu K N O6'
_chemical_formula_sum            'C11 H15 Cl Cu K N O6'
_chemical_formula_weight         395.33
_chemical_name_common            jaa29_0ma
_chemical_name_systematic        'K[(C11H11NO4)CuCl] 2(H2O)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.754(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1219(6)
_cell_length_b                   21.1832(13)
_cell_length_c                   6.8152(3)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.30
_cell_volume                     1407.66(13)
_computing_cell_refinement       'Bruker APEX2 v. 2014.11'
_computing_data_collection       'Bruker APEX2 v. 2014.11'
_computing_data_reduction        'Bruker APEX2 v. 2014.11'
_computing_molecular_graphics    Diamond
_computing_publication_material  CIFTAB
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0082
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            26759
_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         25.371
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       rod
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0180
_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^)+(0.0144P)^2^+3.0642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1261
_reflns_number_total             1299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jaa29_0ma.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348032
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.866
_shelx_res_checksum              28427
_shelx_hkl_checksum              27576