#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/60/2016086.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_2016086
loop_
_publ_author_name
'Redhammer, Günther J.'
'Roth, Georg'
'Amthauer, Georg'
_publ_section_title
;
 Ca₃GeO₄Cl₂ with a norbergite-like structure
;
_journal_coeditor_code           EM3006
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i69
_journal_page_last               i72
_journal_paper_doi               10.1107/S0108270107030478
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Ca3 Ge O4 Cl2'
_chemical_formula_moiety         'Ca3 Cl2 Ge O4'
_chemical_formula_sum            'Ca3 Cl2 Ge O4'
_chemical_formula_weight         327.73
_chemical_name_systematic
;
tricalcium monogermanate dichloride
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7045(8)
_cell_length_b                   10.3432(7)
_cell_length_c                   5.7082(4)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.8
_cell_volume                     691.05(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001) [or APEX2?]'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Version 1.70.01; Farrugia 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method
'rotation, ω scans at 4 different φ positions'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7796
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.372
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(via equivalents using X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.512
_refine_ls_extinction_coef       0.0324(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0302P)²+0.5214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                880
_reflns_number_total             908
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            em3006.cif
_cod_data_source_block           I
_cod_database_code               2016086
_cod_database_fobs_code          2016086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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_refinement_flags
_atom_site_occupancy
Ge Ge1 0.27873(3) 0.25 0.17883(6) 0.00980(15) Uani d S 1
Ca Ca1 0.33637(4) 0.08012(4) 0.61786(8) 0.01406(16) Uani d . 1
Ca Ca2 0.03976(6) 0.25 0.39747(12) 0.01485(18) Uani d S 1
Cl Cl1 0.07046(6) 0.06716(7) 0.75132(13) 0.0294(2) Uani d . 1
O O1 0.19748(15) 0.11792(16) 0.2774(3) 0.0143(3) Uani d . 1
O O2 0.3352(2) 0.25 -0.1034(4) 0.0147(5) Uani d S 1
O O3 0.3966(2) 0.25 0.3725(4) 0.0129(5) Uani d S 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ge1 0.0098(2) 0.0103(2) 0.0094(2) 0 0.00101(12) 0
Ca1 0.0189(3) 0.0108(2) 0.0124(3) -0.00092(17) 0.00031(18) 0.00070(16)
Ca2 0.0103(3) 0.0200(4) 0.0142(3) 0 -0.0004(2) 0
Cl1 0.0243(4) 0.0374(4) 0.0264(4) 0.0121(3) 0.0068(3) 0.0170(3)
O1 0.0140(8) 0.0122(8) 0.0166(8) -0.0031(6) 0.0036(7) -0.0003(7)
O2 0.0179(12) 0.0150(11) 0.0112(11) 0 0.0037(9) 0
O3 0.0120(11) 0.0154(12) 0.0113(11) 0 -0.0021(9) 0
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'
Ca Ca 0.2262 0.3064 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O2 Ge1 O1 . . 120.11(7) yes
O1 Ge1 O1 8_565 . 102.07(11) yes
O2 Ge1 O3 . . 106.40(11) yes
O1 Ge1 O3 . . 102.83(7) yes
O1 Ca1 O3 2 . 164.03(7) ?
O1 Ca1 O2 2 1_556 113.43(6) ?
O3 Ca1 O2 . 1_556 81.25(6) ?
O1 Ca1 O1 2 . 109.27(4) ?
O3 Ca1 O1 . . 67.97(7) ?
O2 Ca1 O1 1_556 . 113.08(7) ?
O1 Ca1 Cl1 2 2_554 82.96(5) ?
O3 Ca1 Cl1 . 2_554 81.11(5) ?
O2 Ca1 Cl1 1_556 2_554 154.73(6) ?
O1 Ca1 Cl1 . 2_554 76.36(4) ?
O1 Ca1 Cl1 2 6_657 91.16(5) ?
O3 Ca1 Cl1 . 6_657 84.44(6) ?
O2 Ca1 Cl1 1_556 6_657 82.20(6) ?
O1 Ca1 Cl1 . 6_657 144.83(4) ?
Cl1 Ca1 Cl1 2_554 6_657 78.22(3) ?
O3 Ca2 O1 6_556 8_565 111.93(7) ?
O3 Ca2 O1 6_556 . 111.93(7) ?
O1 Ca2 O1 8_565 . 69.50(8) ?
O3 Ca2 O2 6_556 6_556 68.74(8) ?
O1 Ca2 O2 8_565 6_556 144.83(4) ?
O1 Ca2 O2 . 6_556 144.83(4) ?
O3 Ca2 Cl1 6_556 8_565 125.78(4) ?
O1 Ca2 Cl1 8_565 8_565 73.83(5) ?
O1 Ca2 Cl1 . 8_565 119.62(5) ?
O2 Ca2 Cl1 6_556 8_565 78.26(4) ?
O3 Ca2 Cl1 6_556 . 125.78(4) ?
O1 Ca2 Cl1 8_565 . 119.62(5) ?
O1 Ca2 Cl1 . . 73.83(5) ?
O2 Ca2 Cl1 6_556 . 78.26(4) ?
Cl1 Ca2 Cl1 8_565 . 85.34(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ge1 O2 . 1.742(2) yes
Ge1 O1 8_565 1.7570(17) no
Ge1 O1 . 1.7570(17) yes
Ge1 O3 . 1.767(2) yes
Ca1 O1 2 2.2764(18) yes
Ca1 O3 . 2.3549(16) yes
Ca1 O2 1_556 2.3703(16) yes
Ca1 O1 . 2.5638(19) yes
Ca1 Cl1 2_554 2.8084(8) yes
Ca1 Cl1 6_657 2.8429(9) yes
Ca2 O3 6_556 2.277(2) yes
Ca2 O1 8_565 2.3967(18) no
Ca2 O1 . 2.3967(18) yes
Ca2 O2 6_556 2.667(3) yes
Ca2 Cl1 8_565 2.7903(8) yes
Ca2 Cl1 . 2.7903(8) no
