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_4348040
_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         '0.5(C27 H34 Co2 K4 N2 O24), 1.52(H2 O)'
_chemical_formula_sum            'C13.5 H20.04 Co K2 N O13.52'
_chemical_formula_weight         549.79
_chemical_name_systematic        'K2[(C13H9NO8)Co(0.5(OCH3))] 4(H2O)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.296(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.901(5)
_cell_length_b                   7.4450(17)
_cell_length_c                   13.408(3)
_cell_measurement_reflns_used    5877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.566
_cell_measurement_theta_min      3.187
_cell_volume                     1976.6(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker AXS APEX II CCD'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker AXS APEX II CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24859
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.647
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.523
_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 0.1377 before and 0.0638 after correction.
 The Ratio of minimum to maximum transmission is 0.73.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 24859 reflections, Rint = 0.0587
 (10005 with I > 3sig(I), Rint = 0.0480)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1107
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.425
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0522P)^2^+15.1626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2872
_reflns_number_total             3260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JA006S.cif
_cod_data_source_block           twin4
_cod_original_cell_volume        1976.7(8)
_cod_original_formula_sum        'C13.50 H20.04 Co K2 N O13.52'
_cod_database_code               4348040
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.965(5) 0.035(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H,H) groups
3. Restrained distances
 O6-H6B = O6-H6A
 0.84 with sigma of 0.02
 O7-H7
 0.84 with sigma of 0.02
4. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H3B(0.5) H3C(0.5) C12(0.25)
 H12B(0.125) H12D(0.125) H12C(0.125) H12A(0.125) H12E(0.125) H12F(0.125)
 O9B(0.24) O9A(0.52)
5.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7A), C6(H6)
5.c Disordered Me refined with riding coordinates:
 C12(H12B,H12D,H12C,H12A,H12E,H12F)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              46955
_shelx_hkl_checksum              22078
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'