Crystal Chemistry of Stanfieldite, Ca7M2Mg9(PO4)12 (M = Ca, Mg, Fe2+), a Structural Base of Ca3Mg3(PO4)4 Phosphors
Britvin, Sergey N.; Krzhizhanovskaya, Maria G.; Bocharov, Vladimir N.; Obolonskaya, Edita V.; Crystals 10 (2020) 464–; doi:10.3390/cryst10060464

data_1558499
_publ_section_title
;
 Crystal Chemistry of Stanfieldite, Ca7M2Mg9(PO4)12 (M = Ca, Mg, Fe2+), a
 Structural Base of Ca3Mg3(PO4)4 Phosphors
;
_journal_issue                   6
_journal_name_full               Crystals
_journal_page_first              464
_journal_paper_doi               10.3390/cryst10060464
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         '0.25(Ca31.87 Fe2.26 Mg37.88 O192 P48)'
_chemical_formula_structural     Ca7(Ca,Mg,Fe)2(Mg,Fe)9(PO4)12
_chemical_formula_sum            'Ca7.97 Fe0.56 Mg9.47 O48 P12'
_chemical_formula_weight         1720.75
_chemical_name_mineral           Stanfieldite
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.954(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7973(4)
_cell_length_b                   9.9833(2)
_cell_length_c                   17.0522(3)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      36.0590
_cell_measurement_theta_min      3.3820
_cell_volume                     3822.53(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 32.4192
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -106.00 -37.00   0.50   75.00    --  -36.45 -57.00 -90.00  138
  2  \w   -115.00 -72.00   0.50   75.00    --  -36.45 178.00 120.00   86
  3  \w     30.00 107.00   0.50   75.00    --   37.54  57.00 150.00  154
  4  \w    -20.00  78.00   0.50   75.00    --   37.54 -99.00  90.00  196
  5  \w     39.00 107.00   0.50   75.00    --   37.54  57.00-150.00  136
  6  \w     39.00  66.00   0.50   75.00    --   37.54  38.00 -60.00   54
  7  \w     -4.00  59.50   0.50   75.00    --   37.54 -99.00 -30.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0123113000
_diffrn_orient_matrix_UB_12      -0.0502305000
_diffrn_orient_matrix_UB_13      0.0274047000
_diffrn_orient_matrix_UB_21      0.0054982000
_diffrn_orient_matrix_UB_22      -0.0407083000
_diffrn_orient_matrix_UB_23      -0.0320399000
_diffrn_orient_matrix_UB_31      0.0285717000
_diffrn_orient_matrix_UB_32      0.0294808000
_diffrn_orient_matrix_UB_33      0.0024066000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18163
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3407
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5420
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3949
_reflns_number_total             5420
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9483\% 
 around [-0.06 1.00 0.01] (reciprocal) or [-0.01 1.00 0.00] (direct)
;
_cod_data_source_file            S1.cif
_cod_data_source_block           Stanfieldite_Brahin
_cod_database_code               1558499
_olex2_refinement_description
;
1. Shared sites
{Mg1, Fe1}
{Mg2, Fe2}
{Mg3, Fe3}
{Mg4, Fe4}
{Mg5, Fe5}
{Ca5A, Mg5A, Fe5A}
2. Uiso/Uaniso restraints and constraints
Uanis(Mg1) = Uanis(Fe1)
Uanis(Mg2) = Uanis(Fe2)
Uanis(Mg3) = Uanis(Fe3)
Uanis(Mg4) = Uanis(Fe4)
Uanis(Mg5) = Uanis(Fe5)
Uanis(Ca5A) = Uanis(Mg5A) = Uanis(Fe5A)
3. Others
 1*[Sof(Ca5A)]+1*[Sof(Mg5A)]+1*[Sof(Fe5A)]=1 with esd of 0.01
 2*[Sof(Ca5A)]+2*[Sof(Mg5A)]+2*[Sof(Fe5A)]=2 with esd of 0.01
 Sof(Fe1)=0.5*(1-FVAR(2))
 Sof(Mg1)=0.5*FVAR(2)
 Sof(Fe2)=1-FVAR(2)
 Sof(Mg2)=FVAR(2)
 Sof(Fe3)=1-FVAR(3)
 Sof(Mg3)=FVAR(3)
 Sof(Fe4)=1-FVAR(4)
 Sof(Mg4)=FVAR(4)
 Sof(Fe5)=1-FVAR(5)
 Sof(Mg5)=FVAR(5)
;
_shelx_res_checksum              40933
_shelx_hkl_checksum              4076
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.929
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2