Solvothermal synthesis, structure and physical properties of Cs[Cr(en)2MSe4] (M = Ge, Sn) with [MSe4](4-) tetrahedra as chelating ligand.
Wang, Yingqi; Wang, Ruiqi; Liu, Qinglong; Lai, Xiaofang; Zhang, Xian; Chen, Haijie; Zheng, Chong; Lin, Jianhua; Huang, Fuqiang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9097–9102; doi:10.1039/c6dt00233a

data_7039045
_publ_section_title
;
 Solvothermal synthesis, structure and physical properties of
 Cs[Cr(en)2MSe4] (M = Ge, Sn) with [MSe4](4-) tetrahedra as chelating
 ligand.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9097
_journal_page_last               9102
_journal_paper_doi               10.1039/c6dt00233a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C4 H16 Cr Cs Ge N4 Se4'
_chemical_formula_sum            'C4 H16 Cr Cs Ge N4 Se4'
_chemical_formula_weight         693.57
_chemical_name_systematic        CsCr(en)2GeSe4
_chemical_properties_physical    Moisture-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-18 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.359(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3115(6)
_cell_length_b                   12.3519(6)
_cell_length_c                   11.4514(5)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      28.8890
_cell_measurement_theta_min      3.9190
_cell_volume                     1597.22(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(1)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5886
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    13.903
_exptl_absorpt_correction_T_max  0.4892
_exptl_absorpt_correction_T_min  0.3370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethylenediamine'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                2568
_reflns_number_total             3122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00233a2.cif
_cod_data_source_block           CsCrGeSe4en2
_cod_depositor_comments
'Adding full bibliography for 7039045--7039046.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7039045