Improved synthesis and characterization of the copper Lyonsite-type compound Cu4−xMo3O12
Raw, Adam D.; Ibers, James A.; Poeppelmeier, Kenneth R.; Journal of Solid State Chemistry 200 (2013) 165–169; doi:10.1016/j.jssc.2013.01.017

data_1562704
_publ_section_title
;
 Improved synthesis and characterization of the copper Lyonsite-type
 compound Cu4&#x2212;xMo3O12
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              165
_journal_page_last               169
_journal_paper_doi               10.1016/j.jssc.2013.01.017
_journal_volume                  200
_journal_year                    2013
_chemical_formula_moiety         'Cu3.8(2) Mo3 O12'
_chemical_formula_sum            'Cu3.83 Mo3 O12'
_chemical_formula_weight         723.34
_chemical_name_common            'copper molybdate lyonsite'
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.99720(10)
_cell_length_b                   11.0259(3)
_cell_length_c                   17.4912(5)
_cell_measurement_reflns_used    24943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.99
_cell_measurement_theta_min      3.7
_cell_volume                     963.74(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2009)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f 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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24943
_diffrn_reflns_theta_full        40.99
_diffrn_reflns_theta_max         40.99
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    12.137
_exptl_absorpt_correction_T_max  0.4114
_exptl_absorpt_correction_T_min  0.2739
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed, SADABS (Sheldrick, 2008b)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1333
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.756
_refine_diff_density_min         -2.545
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(16)
_refine_ls_extinction_coef       0.0030(3)
_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   1.499
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.336
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0203P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                5824
_reflns_number_total             5913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-200-165.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               1562704