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_7225881
_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 ad
_chemical_formula_moiety         'C14 H32 N2 O23 Sm3, B O40 W12, 12(H2 O)'
_chemical_formula_sum            'C14 H56 B N2 O75 Sm3 W12'
_chemical_formula_weight         4120.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.825(2)
_cell_length_b                   11.9982(7)
_cell_length_c                   17.1452(9)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3830
_cell_measurement_theta_min      2.3633
_cell_volume                     7369.6(7)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2014)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2014)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2014)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2014)'
_computing_structure_refinement  '<i>SHELXL-2014/7</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 0.997
_diffrn_measured_fraction_theta_max 0.988
_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  0.0762
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            132651
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         29.416
_diffrn_reflns_theta_min         1.697
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.118
_exptl_absorpt_correction_T_max  0.23
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             7332
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.097
_exptl_transmission_factor_max   0.244
_exptl_transmission_factor_min   0.071
_refine_diff_density_max         3.596
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.316
_refine_ls_abs_structure_details
;
 Flack x determined using 7466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         19873
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0254P)^2^+60.6624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                17950
_reflns_number_total             19873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01183g2.cif
_cod_data_source_block           jtm481a_a
_cod_depositor_comments
'Adding full bibliography for 7225877--7225882.cif.'
_cod_original_cell_volume        7369.7(7)
_cod_database_code               7225881
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.099
_shelx_estimated_absorpt_t_max   0.234
_shelx_res_checksum              20051
_solvent_exptl_crystal_recrystallization_method water