Synthesis and structural characterization of the first neptunium based metal-organic frameworks incorporating {Np<sub>6</sub>O<sub>8</sub>} hexanuclear clusters.
Martin, N. P.; März, J; Feuchter, H.; Duval, S.; Roussel, P.; Henry, N.; Ikeda-Ohno, A; Loiseau, T.; Volkringer, C.; Chemical communications (Cambridge, England) 54 (2018) 6979–6982; doi:10.1039/c8cc03121e

data_7121689
_publ_section_title
;
 Synthesis and structural characterization of the first neptunium based
 metal-organic frameworks incorporating {Np<sub>6</sub>O<sub>8</sub>}
 hexanuclear clusters.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6979
_journal_page_last               6982
_journal_paper_doi               10.1039/c8cc03121e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '(Np1 4+)2(C8 O4 H4 2-)2(C3 N1 O1 H7)'
_chemical_formula_sum            'C22 H22 N2 Np O10'
_chemical_formula_weight         711.41
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3450(7)
_cell_length_b                   11.4621(4)
_cell_length_c                   13.3406(6)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    297.31
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.23
_cell_volume                     2299.89(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      297.31
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.580
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.037
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.00031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2029
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0329
_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^)+13.8292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1807
_reflns_number_total             2029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03121e2.cif
_cod_data_source_block           mo_nm8training_0m_a
_cod_depositor_comments
'Adding full bibliography for 7121688--7121693.cif.'
_cod_database_code               7121689
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.849
_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
2. Rigid bond restraints
 C4, C5, C6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C11(H11)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              16583
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'