Isopentatungstate-supported metal carbonyl derivative: synthesis, characterization, and catalytic properties for alkene epoxidation.
Li, Jie; Guo, Jipeng; Jia, Jiage; Ma, Pengtao; Zhang, Dongdi; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6726–6731; doi:10.1039/c6dt00352d

data_7038644
_publ_section_title
;
 Isopentatungstate-supported metal carbonyl derivative: synthesis,
 characterization, and catalytic properties for alkene epoxidation.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6726
_journal_page_last               6731
_journal_paper_doi               10.1039/c6dt00352d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 K O35 Re4 W5, 3(O), 3(C4 H12 N)'
_chemical_formula_sum            'C24 H48 B0 K N3 O38 Re4 W5'
_chemical_formula_weight         2689.80
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-09 deposited with the CCDC.
2016-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8745(8)
_cell_length_b                   19.1737(11)
_cell_length_c                   22.0448(13)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.33
_cell_volume                     5654.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0490
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28702
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.856
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.820
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1377 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.4007.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.693
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         9944
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8190
_reflns_number_total             9944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00352d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7038644.cif.'
_cod_database_code               7038644
_shelx_estimated_absorpt_t_max   0.153
_shelx_estimated_absorpt_t_min   0.117
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              50716
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'