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_4348043
_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 H19 N Na2 Ni O13, H2.5 O, H1.5 O'
_chemical_formula_sum            'C13 H23 N Na2 Ni O15'
_chemical_formula_weight         538.01
_chemical_name_systematic        'Na2[(C13H9NO8)Ni(H2O)] 6(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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                96.831(3)
_cell_angle_beta                 91.503(3)
_cell_angle_gamma                90.596(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2909(16)
_cell_length_b                   10.357(2)
_cell_length_c                   13.365(3)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.656
_cell_measurement_theta_min      2.886
_cell_volume                     1001.6(4)
_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_type            'Bruker AXS APEX II CCD'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker AXS APEX II CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14570
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.657
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1105 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.8840.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0604P)^2^+0.2102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5652
_reflns_number_total             5972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JA008S.cif
_cod_data_source_block           ja008s
_cod_database_code               4348043
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
2. Restrained distances
 O14-H14A = O14-H14 = O15-H15A = O15-H15 = O11-H11B = O11-H11A = O12-H12A =
 O12-H12B = O13-H13E = O13-H13D = O10-H10A = O10-H10B = O9-H9A = O9-H9B
 0.84 with sigma of 0.02
 O15-H15B
 0.84 with sigma of 0.02
 O15-H15A = O14-H14B
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H15(0.5) H15A(0.5) H14B(0.5) H15B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10)
4.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              28512
_shelx_hkl_checksum              56730
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'