#------------------------------------------------------------------------------
#$Date: 2021-11-04 00:37:16 +0200 (Thu, 04 Nov 2021) $
#$Revision: 270266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/40/4004049.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_4004049
loop_
_publ_author_name
'Song, Xiaoyu'
'Schneider, Sarah N.'
'Cheng, Guangming'
'Khoury, Jason F.'
'Jovanovic, Milena'
'Yao, Nan'
'Schoop, Leslie M.'
_publ_section_title
;
 Kinetics and Evolution of Magnetism in Soft-Chemical Synthesis of CrSe2
 from KCrSe2
;
_journal_issue                   20
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8070
_journal_page_last               8078
_journal_paper_doi               10.1021/acs.chemmater.1c02620
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety         '0.5(Cr2 K2 Se4)'
_chemical_formula_sum            'Cr K Se2'
_chemical_formula_weight         249.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5845(2)
_cell_length_b                   3.80120(10)
_cell_length_c                   7.7116(2)
_cell_measurement_reflns_used    3947
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.16
_cell_measurement_theta_min      2.76
_cell_volume                     185.019(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.262
_diffrn_reflns_theta_min         2.755
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.625
_exptl_absorpt_correction_T_max  0.187
_exptl_absorpt_correction_T_min  0.138
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             222
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.0064(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.417
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.417
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0148P)²+0.7047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                314
_reflns_number_total             323
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm1c02620_si_001.cif
_cod_data_source_block           kcrse2
_cod_database_code               4004049
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.187
_shelx_estimated_absorpt_t_min   0.138
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.77273(5) 1.0000 0.81831(4) 0.00699(15) Uani 1 2 d S T P . .
Cr1 Cr 0.5000 1.0000 1.0000 0.00622(18) Uani 1 4 d S T P . .
K1 K 0.5000 0.5000 0.5000 0.0144(2) Uani 1 4 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
_geom_angle_publ_flag
Cr1 Se1 Cr1 95.236(11) 3 3_545 ?
Cr1 Se1 Cr1 95.241(9) 3 . ?
Cr1 Se1 Cr1 95.241(9) 3_545 . ?
Cr1 Se1 K1 164.466(11) 3_545 1_565 ?
Cr1 Se1 K1 164.481(13) . 3 ?
Cr1 Se1 K1 95.202(8) 3 3 ?
Cr1 Se1 K1 95.221(8) . 1_565 ?
Cr1 Se1 K1 164.466(11) 3 . ?
Cr1 Se1 K1 95.202(8) 3_545 3 ?
Cr1 Se1 K1 95.208(3) 3_545 . ?
Cr1 Se1 K1 95.221(8) . . ?
Cr1 Se1 K1 95.208(3) 3 1_565 ?
K1 Se1 K1 72.411(7) . 3 ?
K1 Se1 K1 72.417(7) . 1_565 ?
K1 Se1 K1 72.411(7) 1_565 3 ?
Se1 Cr1 Se1 180.0 7_677 3_445 ?
Se1 Cr1 Se1 84.758(9) 3_455 5_677 ?
Se1 Cr1 Se1 95.242(9) 3_455 . ?
Se1 Cr1 Se1 95.236(11) 7_677 7_667 ?
Se1 Cr1 Se1 95.242(9) 3_445 . ?
Se1 Cr1 Se1 84.764(11) 3_445 7_667 ?
Se1 Cr1 Se1 95.242(9) 7_667 5_677 ?
Se1 Cr1 Se1 84.764(11) 7_677 3_455 ?
Se1 Cr1 Se1 84.758(9) 7_677 . ?
Se1 Cr1 Se1 95.236(11) 3_445 3_455 ?
Se1 Cr1 Se1 84.758(9) 7_667 . ?
Se1 Cr1 Se1 180.0 7_667 3_455 ?
Se1 Cr1 Se1 180.000(14) 5_677 . ?
Se1 Cr1 Se1 84.758(9) 3_445 5_677 ?
Se1 Cr1 Se1 95.242(9) 7_677 5_677 ?
Se1 K1 Se1 180.0 . 5_666 ?
Se1 K1 Se1 72.411(7) 5_676 7_666 ?
Se1 K1 Se1 72.411(7) 1_545 3_445 ?
Se1 K1 Se1 107.583(7) . 5_676 ?
Se1 K1 Se1 107.589(7) 5_666 3_445 ?
Se1 K1 Se1 72.416(7) 5_666 5_676 ?
Se1 K1 Se1 72.411(7) 5_666 7_666 ?
Se1 K1 Se1 72.417(7) . 1_545 ?
Se1 K1 Se1 72.411(7) . 3_445 ?
Se1 K1 Se1 107.584(7) 5_666 1_545 ?
Se1 K1 Se1 107.589(7) 5_676 3_445 ?
Se1 K1 Se1 180.0 5_676 1_545 ?
Se1 K1 Se1 180.0 7_666 3_445 ?
Se1 K1 Se1 107.589(7) . 7_666 ?
Se1 K1 Se1 107.589(7) 1_545 7_666 ?
Se1 K1 K1 53.792(4) . 1_565 ?
Se1 K1 K1 126.194(6) 1_545 3_455 ?
Se1 K1 K1 89.991(5) 5_666 3_545 ?
Se1 K1 K1 126.208(4) 5_666 1_565 ?
Se1 K1 K1 89.991(5) 1_545 3_445 ?
Se1 K1 K1 126.208(4) 1_545 1_565 ?
Se1 K1 K1 126.216(5) 3_445 3_545 ?
Se1 K1 K1 90.0 7_666 1_565 ?
Se1 K1 K1 53.806(6) 5_666 3_445 ?
Se1 K1 K1 90.0 3_445 1_565 ?
Se1 K1 K1 53.784(5) 3_445 3_445 ?
Se1 K1 K1 126.208(4) . 1_545 ?
Se1 K1 K1 53.806(6) 1_545 3_545 ?
Se1 K1 K1 53.792(4) 5_666 1_545 ?
Se1 K1 K1 90.009(5) 5_666 3_455 ?
Se1 K1 K1 126.208(4) 5_676 1_545 ?
Se1 K1 K1 53.784(5) 3_445 3_455 ?
Se1 K1 K1 53.792(4) 1_545 1_545 ?
Se1 K1 K1 90.009(5) 5_676 3_445 ?
Se1 K1 K1 90.0 7_666 1_545 ?
Se1 K1 K1 126.216(5) 7_666 3_445 ?
Se1 K1 K1 90.0 3_445 1_545 ?
Se1 K1 K1 90.009(5) . 3_545 ?
Se1 K1 K1 53.805(6) . 3 ?
Se1 K1 K1 126.194(6) 5_676 3_545 ?
Se1 K1 K1 126.194(6) 5_666 3 ?
Se1 K1 K1 53.784(5) 7_666 3_545 ?
Se1 K1 K1 89.991(5) 5_676 3 ?
Se1 K1 K1 89.991(5) . 3_455 ?
Se1 K1 K1 90.009(5) 1_545 3 ?
Se1 K1 K1 53.806(6) 5_676 3_455 ?
Se1 K1 K1 53.784(5) 7_666 3 ?
Se1 K1 K1 126.216(5) 7_666 3_455 ?
Se1 K1 K1 126.216(5) 3_445 3 ?
Se1 K1 K1 126.195(6) . 3_445 ?
Se1 K1 K1 53.792(4) 5_676 1_565 ?
K1 K1 K1 119.998(1) 1_565 3_545 ?
K1 K1 K1 180.0 1_565 1_545 ?
K1 K1 K1 120.005(2) 3 3_455 ?
K1 K1 K1 60.002(1) 1_545 3_545 ?
K1 K1 K1 60.002(1) 1_565 3_455 ?
K1 K1 K1 59.995(2) 3 3_545 ?
K1 K1 K1 60.002(1) 1_545 3_445 ?
K1 K1 K1 120.005(2) 3_445 3_545 ?
K1 K1 K1 119.998(1) 1_565 3_445 ?
K1 K1 K1 180.0 3 3_445 ?
K1 K1 K1 119.998(1) 1_545 3_455 ?
K1 K1 K1 60.002(1) 1_565 3 ?
K1 K1 K1 59.995(2) 3_445 3_455 ?
K1 K1 K1 119.998(1) 1_545 3 ?
K1 K1 K1 180.0 3_545 3_455 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 Cr1 2.5730(2) 3 ?
Se1 Cr1 2.5730(2) 3_545 ?
Se1 Cr1 2.5732(3) . ?
Se1 K1 3.2174(3) . ?
Se1 K1 3.2183(3) 3 ?
Se1 K1 3.2174(3) 1_565 ?
Cr1 Se1 2.5730(2) 7_677 ?
Cr1 Se1 2.5730(2) 7_667 ?
Cr1 Se1 2.5730(2) 3_455 ?
Cr1 Se1 2.5730(2) 3_445 ?
Cr1 Se1 2.5731(3) 5_677 ?
K1 Se1 3.2174(3) 5_666 ?
K1 Se1 3.2174(3) 1_545 ?
K1 Se1 3.2183(3) 7_666 ?
K1 Se1 3.2174(3) 5_676 ?
K1 Se1 3.2183(3) 3_445 ?
K1 K1 3.80147(9) 3_455 ?
K1 K1 3.80147(9) 3_545 ?
K1 K1 3.80147(9) 3_445 ?
K1 K1 3.80120(10) 1_545 ?
K1 K1 3.80147(9) 3 ?
K1 K1 3.80120(10) 1_565 ?
