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_4342418
_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         'Ni O6 Pb Se2'
_chemical_formula_sum            'Ni O6 Pb Se2'
_chemical_formula_weight         519.82
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4715(4)
_cell_length_b                   9.1963(6)
_cell_length_c                   11.4436(9)
_cell_measurement_reflns_used    2417
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      3.56
_cell_volume                     575.81(7)
_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 0.971
_diffrn_measured_fraction_theta_max 0.962
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2345
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.945
_diffrn_reflns_theta_min         3.561
_exptl_absorpt_coefficient_mu    45.074
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.996
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.403(9)
_refine_ls_extinction_coef       0.00091(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         686
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0141
_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^)+(0.0151P)^2^+1.0537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0346
_refine_ls_wR_factor_ref         0.0346
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                683
_reflns_number_total             686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic503055v_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4342415--4342418.cif.'
_cod_database_code               4342418