#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:55:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179518 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/15/4341535.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4341535
loop_
_publ_author_name
'Zhang, Guodong'
'Li, Peizhou'
'Ding, Junfeng'
'Liu, Yi'
'Xiong, Wei-Wei'
'Nie, Lina'
'Wu, Tom'
'Zhao, Yanli'
'Tok, Alfred Iing Yoong'
'Zhang, Qichun'
_publ_section_title
;
 Surfactant-thermal syntheses, structures, and magnetic properties of
 mn-ge-sulfides/selenides.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10248
_journal_page_last               10256
_journal_paper_doi               10.1021/ic501282d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C7 H20 Ge Mn N4 O Se4'
_chemical_formula_weight         619.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   no
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.438(5)
_cell_angle_beta                 86.152(4)
_cell_angle_gamma                75.290(4)
_cell_formula_units_Z            2
_cell_length_a                   6.4841(8)
_cell_length_b                   9.3282(14)
_cell_length_c                   14.586(2)
_cell_measurement_temperature    293(2)
_cell_volume                     849.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9654
_diffrn_reflns_theta_full        29.47
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    11.074
_exptl_absorpt_correction_T_max  0.2155
_exptl_absorpt_correction_T_min  0.1167
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.020
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.422
_refine_ls_extinction_coef       0.00156(7)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    no
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0764P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                3371
_reflns_number_total             4664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501282d_si_006.cif
_cod_data_source_block           x2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341535
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
Se1 Se 0.06519(12) 0.16226(9) 0.66881(6) 0.0109(2) Uani 1 1 d
Se2 Se -0.06865(12) 0.42256(9) 0.85446(6) 0.00971(19) Uani 1 1 d
Se3 Se 0.49282(12) 0.13779(9) 0.85122(6) 0.01011(19) Uani 1 1 d
Se4 Se -0.59707(12) 0.45499(9) 0.67907(6) 0.01004(19) Uani 1 1 d
Ge Ge 0.22367(12) 0.29296(9) 0.76316(6) 0.00748(19) Uani 1 1 d
Mn Mn -0.27392(17) 0.28755(13) 0.76038(8) 0.0093(3) Uani 1 1 d
C1 C 0.0305(13) 0.1726(10) 0.1106(6) 0.0176(19) Uani 1 1 d
C2 C 0.1332(12) 0.2482(10) 0.3506(7) 0.020(2) Uani 1 1 d
C3 C 0.1431(13) 0.3621(10) 0.4190(6) 0.0182(19) Uani 1 1 d
C4 C 0.3463(13) 0.2074(10) 0.2973(6) 0.0172(19) Uani 1 1 d
C5 C 0.5055(12) 0.2018(9) 0.4441(6) 0.0111(16) Uani 1 1 d
C6 C -0.3653(12) 0.2786(10) 0.0751(6) 0.0138(17) Uani 1 1 d
C7 C -0.2018(12) 0.1846(9) 0.1410(5) 0.0117(16) Uani 1 1 d
N1 N 0.0763(10) 0.1179(8) 0.0147(5) 0.0169(16) Uani 1 1 d
N2 N 0.3376(11) 0.3049(8) 0.4741(5) 0.0165(15) Uani 1 1 d
N3 N 0.5170(10) 0.1496(8) 0.3622(5) 0.0149(15) Uani 1 1 d
N4 N -0.3651(11) 0.4381(8) 0.0675(5) 0.0177(16) Uani 1 1 d
O O 0.6874(13) 0.1416(11) 0.5094(7) 0.065(3) Uani 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Se Se -0.0929 2.2259 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Ge Se1 Mn 82.60(4) . .
Ge Se2 Mn 82.06(4) . .
Ge Se3 Mn 82.80(4) . 1_655
Ge Se4 Mn 82.20(4) 1_455 .
Se3 Ge Se1 113.20(4) . .
Se3 Ge Se4 102.96(4) . 1_655
Se1 Ge Se4 113.10(4) . 1_655
Se3 Ge Se2 112.83(4) . .
Se1 Ge Se2 103.17(4) . .
Se4 Ge Se2 111.93(4) 1_655 .
Se3 Mn Se1 121.82(5) 1_455 .
Se3 Mn Se4 91.84(4) 1_455 .
Se1 Mn Se4 121.12(6) . .
Se3 Mn Se2 116.74(5) 1_455 .
Se1 Mn Se2 92.16(4) . .
Se4 Mn Se2 115.42(5) . .
N1 C1 C7 110.5(7) . .
C4 C2 C3 108.4(7) . .
N2 C3 C2 109.4(7) . .
N3 C4 C2 109.3(7) . .
N3 C5 N2 122.3(7) . .
N3 C5 O 120.0(7) . .
N2 C5 O 117.7(7) . .
N4 C6 C7 113.2(7) . .
C1 C7 C6 115.2(7) . .
C5 N2 C3 122.1(7) . .
C5 N3 C4 121.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Ge 2.3514(11) .
Se1 Mn 2.5561(13) .
Se2 Ge 2.3625(10) .
Se2 Mn 2.5714(14) .
Se3 Ge 2.3480(11) .
Se3 Mn 2.5503(15) 1_655
Se4 Ge 2.3550(12) 1_455
Se4 Mn 2.5717(14) .
Ge Se4 2.3550(12) 1_655
Mn Se3 2.5503(15) 1_455
C1 N1 1.511(10) .
C1 C7 1.520(11) .
C2 C4 1.515(12) .
C2 C3 1.529(12) .
C3 N2 1.498(11) .
C4 N3 1.473(10) .
C5 N3 1.316(10) .
C5 N2 1.331(10) .
C5 O 1.531(11) .
C6 N4 1.484(11) .
C6 C7 1.532(11) .
