Structural scope of six new layered to pillar-layered hybrid inorganic‒organic networks bearing [BW12O40]5−and lanthanoid-cluster; database study toward ligand role in assemblies
Najafi, Atefeh; Mirzaei, Masoud; Mague, Joel T.; CrystEngComm 18 (2016) 6724–; doi:10.1039/C6CE01183G

data_7225879
_publ_section_title
;
 Structural scope of six new layered to pillar-layered hybrid
 inorganic--organic networks bearing [BW12O40]5&#x2212;and
 lanthanoid-cluster; database study toward ligand role in assemblies
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6724
_journal_paper_doi               10.1039/C6CE01183G
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H44 N4 Nd4 O32, K, B O40 W12, 2(H2 O)'
_chemical_formula_sum            'C28 H48 B K N4 Nd4 O74 W12'
_chemical_formula_weight         4457.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-11 deposited with the CCDC.
2016-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.930(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4412(13)
_cell_length_b                   15.5369(7)
_cell_length_c                   21.9253(10)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0516
_cell_measurement_theta_min      2.3963
_cell_volume                     7592.6(6)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2015)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2015)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2015)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2015)'
_computing_structure_refinement  '<i>SHELXL</i> (Sheldrick, 2015a)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69377
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        28.750
_diffrn_reflns_theta_max         29.150
_diffrn_reflns_theta_min         1.827
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.962
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2015)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    3.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             7952
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   0.697
_exptl_transmission_factor_min   0.149
_refine_diff_density_max         18.708
_refine_diff_density_min         -10.823
_refine_diff_density_rms         0.550
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         19864
_refine_ls_number_restraints     638
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0048P)^2^+1546.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                16177
_reflns_number_total             19864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01183g2.cif
_cod_data_source_block           JTM461a_0m_b
_cod_depositor_comments
'Adding full bibliography for 7225877--7225882.cif.'
_cod_database_code               7225879
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.176
_shelx_estimated_absorpt_t_max   0.527
_shelx_res_checksum              83011
_solvent_exptl_crystal_recrystallization_method water