A Ni-containing decaniobate incorporating organic ligands: synthesis, structure, and catalysis for allylic alcohol epoxidation
Li, Li; Niu, Yanjun; Dong, Kaili; Ma, Pengtao; Zhang, Chao; Niu, Jingyang; Wang, Jingping; RSC Adv. 7 (2017) 28696–; doi:10.1039/C7RA03254D

data_7228353
_publ_section_title
;
 A Ni-containing decaniobate incorporating organic ligands: synthesis,
 structure, and catalysis for allylic alcohol epoxidation
;
_journal_issue                   46
_journal_name_full               'RSC Adv.'
_journal_page_first              28696
_journal_paper_doi               10.1039/C7RA03254D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C4 H16 N4 Na8 Nb10 Ni3 O58, 2(O)'
_chemical_formula_sum            'C4 H72 N4 Na8 Nb10 Ni3 O60'
_chemical_formula_weight         2425.80
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-09 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                61.8590(10)
_cell_angle_beta                 63.6420(10)
_cell_angle_gamma                61.2230(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5635(8)
_cell_length_b                   12.9279(9)
_cell_length_c                   13.1370(9)
_cell_measurement_reflns_used    3147
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.19
_cell_volume                     1582.83(19)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0193
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8189
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         1.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.783
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0592 before and 0.0311 after correction.
The Ratio of minimum to maximum transmission is 0.7994.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0461P)^2^+9.6880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4475
_reflns_number_total             5578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra03254d2.cif
_cod_data_source_block           njy1
_cod_database_code               7228353
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.426
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D)
;
_shelx_res_checksum              2143
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'