A new Keggin-like niobium-phosphate cluster that reacts reversibly with hydrogen peroxide.
Son, Jung-Ho; Casey, William H.; Chemical communications (Cambridge, England) 51 (2015) 12744–12747; doi:10.1039/c5cc03782d

data_7117582
_publ_section_title
;
 A new Keggin-like niobium-phosphate cluster that reacts reversibly with
 hydrogen peroxide.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12744
_journal_page_last               12747
_journal_paper_doi               10.1039/c5cc03782d
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C36 H108 N9 Nb9 O69.5 P5'
_chemical_formula_weight         2770.35
_chemical_name_systematic        'tetramethyalmmonium nonaniobopentaphosphate'
_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_method           SHELXL-2014/7
_audit_update_record
;
2015-05-02 deposited with the CCDC.
2015-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7420(10)
_cell_angle_gamma                90
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_cell_length_b                   15.4386(12)
_cell_length_c                   24.5428(19)
_cell_measurement_reflns_used    9318
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.23
_cell_volume                     10357.2(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            118377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       plate
_exptl_crystal_F_000             5548
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.641
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.670
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         23883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.150
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+76.0136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18801
_reflns_number_total             23883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03782d2.cif
_cod_data_source_block           p21c-mulit
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        10357.0(14)
_cod_original_formula_sum        'C36 H108 N9 Nb9 O69.50 P5'
_cod_database_code               7117582
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.528
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              33127