pH Controlled Pathway and Systematic Hydrothermal Phase Diagram for Elaboration of Synthetic Lead Nickel Selenites.
Kovrugin, Vadim M.; Colmont, Marie; Terryn, Christine; Colis, Silviu; Siidra, Oleg I.; Krivovichev, Sergey V.; Mentré, Olivier; Inorganic chemistry 54 (2015) 2425–; doi:10.1021/ic503055v

data_4342417
_publ_section_title
;
 pH Controlled Pathway and Systematic Hydrothermal Phase Diagram for
 Elaboration of Synthetic Lead Nickel Selenites.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2425
_journal_paper_doi               10.1021/ic503055v
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'H2 Ni2 O12 Pb Se4'
_chemical_formula_sum            'H2 Ni2 O12 Pb Se4'
_chemical_formula_weight         834.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 129.524(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6824(10)
_cell_length_b                   5.2692(5)
_cell_length_c                   19.3476(13)
_cell_measurement_reflns_used    2655
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.34
_cell_measurement_theta_min      2.99
_cell_volume                     1075.95(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.821
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5454
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.930
_exptl_absorpt_coefficient_mu    32.668
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    5.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.916
_refine_diff_density_min         -2.912
_refine_diff_density_rms         0.462
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2083
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+23.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1550
_reflns_number_total             2083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic503055v_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4342415--4342418.cif.'
_cod_original_cell_volume        1075.94(16)
_cod_database_code               4342417