Crystallization of phosphomolybdate clusters mediated by copper azole complexes: Influence of pH and temperature
Jency Thomas; Dinesh Kumar; Arunachalam Ramanan; Inorganica Chimica Acta 396 (2013) 126–135; doi:10.1016/j.ica.2012.10.034

data_1513006
_publ_section_title
;
 Crystallization of phosphomolybdate clusters mediated by copper azole
 complexes: Influence of pH and temperature
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              126
_journal_page_last               135
_journal_paper_doi               10.1016/j.ica.2012.10.034
_journal_volume                  396
_journal_year                    2013
_chemical_formula_moiety         'C12 H16 Cu2 Mo5 N8 O26 P2, 3(C3 H5 N2), O'
_chemical_formula_sum            'C21 H31 Cu2 Mo5 N14 O27 P2'
_chemical_formula_weight         1580.34
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.916(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.770(3)
_cell_length_b                   18.565(6)
_cell_length_c                   13.970(5)
_cell_measurement_reflns_used    4546
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.19
_cell_volume                     2164.2(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25393
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    2.550
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.248
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.582
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.582
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.5644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                4795
_reflns_number_total             5598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-126-135-5.cif
_cod_data_source_block           jp41em
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1513006