Unique solubility of polyoxoniobate salts in methanol: coordination to cations and POM methylation
Abramov, Pavel A.; Vicent, Cristian; Kompankov, Nikolay B.; Laricheva, Yuliya A.; Sokolov, Maksim Nailyevich; RSC Adv.  (2016) –; doi:10.1039/C5RA23918D

data_7224055
_publ_section_title
;
 Unique solubility of polyoxoniobate salts in methanol: coordination to
 cations and POM methylation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA23918D
_journal_year                    2016
_chemical_formula_structural     K4[{C10H15Ir}2Nb6O19]*10CH3OH*4H2O
_chemical_formula_sum            'C30 H78 Ir2 K4 Nb6 O33'
_chemical_formula_weight         2065.18
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-11 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.102(3)
_cell_angle_beta                 92.519(3)
_cell_angle_gamma                111.051(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7760(6)
_cell_length_b                   11.8756(7)
_cell_length_c                   14.1839(9)
_cell_measurement_reflns_used    6620
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.10
_cell_volume                     1521.58(17)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18012
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         1.598
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.800
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_description       yellow
_exptl_crystal_F_000             998
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.697
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.628
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0764P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5935
_reflns_number_total             6901
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra23918d2.cif
_cod_data_source_block           18
_cod_original_cell_volume        1521.58(16)
_cod_database_code               7224055
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.722
_shelx_res_checksum              24164