#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/96/2019639.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019639
loop_
_publ_author_name
'Redhammer, Günther J.'
'Tippelt, Gerold'
_publ_section_title
;
 Pyroxene-type compounds NaM³⁺Ge₂O₆, with M = Ga, Mn,
 Sc and In
;
_journal_coeditor_code           EG3165
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614017768
_journal_volume                  70
_journal_year                    2014
_chemical_formula_analytical     'Ge1.9 Mn Na O6 V0.1'
_chemical_formula_iupac          'Na Mn V0.1 Ge1.9 O6'
_chemical_formula_moiety         'Ge1.9 Mn O6 V0.1, 1(Na)'
_chemical_formula_sum            'Ge1.9 Mn Na O6 V0.1'
_chemical_formula_weight         316.945
_chemical_name_common            pyroxene
_chemical_name_systematic
;
Sodium manganese vanadate germanate
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.3818(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9611(13)
_cell_length_b                   8.8630(11)
_cell_length_c                   5.5598(7)
_cell_measurement_reflns_used    2505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.242
_cell_measurement_theta_min      3.135
_cell_volume                     470.92(10)
_computing_cell_refinement       'APEX2 (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'APEX2 (Bruker, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX  (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2012 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method
'rotation, ω scans at four different φ positions'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2505
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         3.135
_exptl_absorpt_coefficient_mu    14.93
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2012)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.748
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0288P)²+2.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                558
_reflns_number_total             585
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            eg3165sup1.cif
_cod_data_source_block           NMnG
_cod_database_code               2019639
_cod_database_fobs_code          2019639
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Na Na1 0 0.30110(18) 0.25 0.0111(3) Uani d 1
Mn Mn1 0 0.90765(7) 0.25 0.00847(16) Uani d 1
Ge Ge1 0.28982(3) 0.09350(3) 0.23556(6) 0.01186(14) Uani d 0.95
V V1 0.28982(3) 0.09350(3) 0.23556(6) 0.01186(14) Uani d 0.05
O O2 0.3585(3) 0.2713(3) 0.3065(5) 0.0233(5) Uani d 1
O O1 0.1080(3) 0.0806(3) 0.1442(5) 0.0188(5) Uani d 1
O O3 0.3622(2) 0.0100(3) 0.0145(4) 0.0183(5) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Na1 O1 . 2 69.81(13)
O1 Na1 O3 . 4 121.84(8)
O1 Na1 O3 2 4 135.32(8)
O1 Na1 O3 . 3_455 135.32(8)
O1 Na1 O3 2 3_455 121.84(8)
O3 Na1 O3 4 3_455 81.93(12)
O1 Na1 O2 . 8_455 73.74(9)
O1 Na1 O2 2 8_455 82.40(9)
O3 Na1 O2 4 8_455 141.16(9)
O3 Na1 O2 3_455 8_455 66.47(8)
O1 Na1 O2 . 7_556 82.40(9)
O1 Na1 O2 2 7_556 73.74(9)
O3 Na1 O2 4 7_556 66.47(8)
O3 Na1 O2 3_455 7_556 141.16(9)
O2 Na1 O2 8_455 7_556 150.88(13)
O1 Na1 O3 . 8_456 158.98(9)
O1 Na1 O3 2 8_456 92.19(8)
O3 Na1 O3 4 8_456 63.62(9)
O3 Na1 O3 3_455 8_456 63.24(5)
O2 Na1 O3 8_455 8_456 115.77(8)
O2 Na1 O3 7_556 8_456 82.13(8)
O1 Na1 O3 . 7 92.19(8)
O1 Na1 O3 2 7 158.98(9)
O3 Na1 O3 4 7 63.24(5)
O3 Na1 O3 3_455 7 63.62(9)
O2 Na1 O3 8_455 7 82.13(8)
O2 Na1 O3 7_556 7 115.77(8)
O3 Na1 O3 8_456 7 107.35(11)
O2 Mn1 O2 3_455 4 103.31(15)
O2 Mn1 O1 3_455 1_565 166.24(11)
O2 Mn1 O1 4 1_565 87.46(10)
O2 Mn1 O1 3_455 2_565 87.46(10)
O2 Mn1 O1 4 2_565 166.24(11)
O1 Mn1 O1 1_565 2_565 83.32(13)
O2 Mn1 O1 3_455 6_566 92.42(10)
O2 Mn1 O1 4 6_566 91.02(11)
O1 Mn1 O1 1_565 6_566 95.97(9)
O1 Mn1 O1 2_565 6_566 79.85(10)
O2 Mn1 O1 3_455 5_565 91.02(11)
O2 Mn1 O1 4 5_565 92.42(10)
O1 Mn1 O1 1_565 5_565 79.85(10)
O1 Mn1 O1 2_565 5_565 95.97(9)
O1 Mn1 O1 6_566 5_565 174.46(13)
O2 Ge1 O1 . . 116.18(12)
O2 Ge1 O3 . . 109.36(12)
O1 Ge1 O3 . . 111.54(11)
O2 Ge1 O3 . 6_556 103.69(12)
O1 Ge1 O3 . 6_556 110.76(11)
O3 Ge1 O3 . 6_556 104.40(8)
Ge1 O3 Ge1 . 6 133.29(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Na1 O1 . 2.383(3)
Na1 O3 4 2.452(3)
Na1 O2 8_455 2.553(3)
Na1 O3 8_456 2.826(3)
Mn1 O2 3_455 1.948(3)
Mn1 O1 1_565 2.052(3)
Mn1 O1 6_566 2.154(3)
Ge1 O2 . 1.719(2)
Ge1 O1 . 1.742(3)
Ge1 O3 . 1.754(2)
Ge1 O3 6_556 1.771(2)
