#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:28:59 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231564 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/33/4003390.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_4003390
loop_
_publ_author_name
'Ashoka Sahadevan, Suchithra'
'Monni, Noemi'
'Abhervé, Alexandre'
'Marongiu, Daniela'
'Sarritzu, Valerio'
'Sestu, Nicola'
'Saba, Michele'
'Mura, Andrea'
'Bongiovanni, Giovanni'
'Cannas, Carla'
'Quochi, Francesco'
'Avarvari, Narcis'
'Mercuri, Maria Laura'
_publ_section_title
;
 Nanosheets of Two-Dimensional Neutral Coordination Polymers Based on
 Near-Infrared-Emitting Lanthanides and a Chlorocyananilate Ligand
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6575
_journal_paper_doi               10.1021/acs.chemmater.8b03399
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety
'Er2 C21 N3 O12 Cl3, C18 H42 N6 O6, C2 H4 Cl4'
_chemical_formula_sum            'C41 H46 Cl7 Er2 N9 O18'
_chemical_formula_weight         1535.54
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.075(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7965(4)
_cell_length_b                   22.5774(8)
_cell_length_c                   17.9680(8)
_cell_measurement_reflns_used    5986
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3050
_cell_measurement_theta_min      3.7490
_cell_volume                     5541.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11988
_diffrn_reflns_theta_full        74.01
_diffrn_reflns_theta_max         74.01
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    9.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5493
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0500
_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/[σ²(Fo²)+(0.0564P)²+43.0565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                4820
_reflns_number_total             5493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm8b03399_si_004.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4003390
_oxdiff_exptl_absorpt_empirical_full_min 0.814
_oxdiff_exptl_absorpt_empirical_full_max 1.585
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_symmetry_equiv_pos_as_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_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
_atom_site_refinement_flags
C1 C 0.3993(4) 0.4999(3) 0.5152(3) 0.0246(11) Uani 1 1 d .
C2 C 0.4790(4) 0.4614(2) 0.5591(3) 0.0249(11) Uani 1 1 d .
C3 C 0.4258(4) 0.5374(3) 0.4601(3) 0.0260(12) Uani 1 1 d .
C4 C 0.0744(4) 0.4548(2) 0.5007(3) 0.0227(11) Uani 1 1 d .
C5 C 0.0789(4) 0.5027(3) 0.5614(3) 0.0225(11) Uani 1 1 d .
C6 C 0.0046(4) 0.5452(3) 0.5576(3) 0.0256(12) Uani 1 1 d .
C7 C 0.2963(4) 0.3072(2) 0.5107(3) 0.0191(10) Uani 1 1 d .
C8 C 0.2133(4) 0.2884(2) 0.5543(3) 0.0206(10) Uani 1 1 d .
C9 C 0.1706(4) 0.2313(3) 0.5394(3) 0.0236(11) Uani 1 1 d .
C10 C 0.3976(5) 0.3431(3) 0.7642(3) 0.0308(13) Uani 1 1 d .
H10 H 0.4271 0.3754 0.7903 0.037 Uiso 1 1 calc R
C11 C 0.3585(9) 0.2399(4) 0.7616(6) 0.082(4) Uani 1 1 d .
H11A H 0.3718 0.2062 0.7940 0.124 Uiso 1 1 calc R
H11B H 0.3838 0.2329 0.7153 0.124 Uiso 1 1 calc R
H11C H 0.2891 0.2462 0.7514 0.124 Uiso 1 1 calc R
C12 C 0.4575(6) 0.2849(4) 0.8732(4) 0.052(2) Uani 1 1 d .
H12A H 0.4553 0.2442 0.8883 0.078 Uiso 1 1 calc R
H12B H 0.4276 0.3092 0.9074 0.078 Uiso 1 1 calc R
H12C H 0.5244 0.2968 0.8736 0.078 Uiso 1 1 calc R
C13 C 0.2830(5) 0.5177(3) 0.7494(3) 0.0293(13) Uani 1 1 d .
H13 H 0.2154 0.5134 0.7393 0.035 Uiso 1 1 calc R
C14 C 0.2537(6) 0.5891(4) 0.8435(5) 0.051(2) Uani 1 1 d .
H14A H 0.2915 0.6139 0.8801 0.077 Uiso 1 1 calc R
H14B H 0.2137 0.5629 0.8683 0.077 Uiso 1 1 calc R
H14C H 0.2125 0.6134 0.8083 0.077 Uiso 1 1 calc R
C15 C 0.4206(5) 0.5657(4) 0.8210(5) 0.0458(18) Uani 1 1 d D
H15A H 0.4323 0.5942 0.8609 0.069 Uiso 1 1 calc R
H15B H 0.4448 0.5808 0.7772 0.069 Uiso 1 1 calc R
H15C H 0.4538 0.5294 0.8365 0.069 Uiso 1 1 calc R
C16 C 0.1471(4) 0.3666(3) 0.7487(3) 0.0291(13) Uani 1 1 d .
H16 H 0.1630 0.3290 0.7330 0.035 Uiso 1 1 calc R
C17 C 0.0804(6) 0.4264(4) 0.8399(5) 0.054(2) Uani 1 1 d .
H17A H 0.0489 0.4203 0.8836 0.080 Uiso 1 1 calc R
H17B H 0.0378 0.4484 0.8031 0.080 Uiso 1 1 calc R
H17C H 0.1401 0.4481 0.8537 0.080 Uiso 1 1 calc R
C18 C 0.0786(7) 0.3168(5) 0.8479(5) 0.064(3) Uani 1 1 d .
H18A H 0.0473 0.3275 0.8904 0.096 Uiso 1 1 calc R
H18B H 0.1376 0.2953 0.8647 0.096 Uiso 1 1 calc R
H18C H 0.0352 0.2925 0.8144 0.096 Uiso 1 1 calc R
N4 N 0.4048(4) 0.2917(3) 0.7979(3) 0.0400(14) Uani 1 1 d .
N5 N 0.3185(4) 0.5549(3) 0.8041(3) 0.0347(12) Uani 1 1 d D
N6 N 0.1023(4) 0.3700(3) 0.8089(3) 0.0404(13) Uani 1 1 d .
O1 O 0.4508(3) 0.43217(19) 0.6111(2) 0.0283(9) Uani 1 1 d .
O2 O 0.3145(3) 0.49404(19) 0.5316(2) 0.0274(9) Uani 1 1 d .
O3 O 0.1432(3) 0.41870(17) 0.5084(2) 0.0264(9) Uani 1 1 d .
O4 O 0.1519(3) 0.49983(19) 0.6109(2) 0.0268(9) Uani 1 1 d .
O5 O 0.3287(3) 0.35843(17) 0.5249(2) 0.0239(8) Uani 1 1 d .
O6 O 0.1879(3) 0.32463(18) 0.5996(2) 0.0250(8) Uani 1 1 d .
O7 O 0.3543(3) 0.3518(2) 0.6999(2) 0.0323(10) Uani 1 1 d .
O8 O 0.3339(3) 0.48853(19) 0.7112(2) 0.0298(9) Uani 1 1 d .
O9 O 0.1693(3) 0.40882(19) 0.7118(2) 0.0287(9) Uani 1 1 d .
Er1 Er 0.27181(2) 0.420497(14) 0.616790(17) 0.01966(12) Uani 1 1 d .
Cl1 Cl 0.3341(4) 0.5792(2) 0.4087(3) 0.0333(9) Uani 0.50 1 d P
Cl2 Cl 0.0114(4) 0.5971(3) 0.6295(4) 0.0465(16) Uani 0.50 1 d P
Cl3 Cl 0.0759(5) 0.2102(3) 0.5876(4) 0.0396(14) Uani 0.50 1 d P
C19 C 0.351(3) 0.573(2) 0.422(3) 0.10(2) Uiso 0.50 1 d P
C20 C 0.008(2) 0.5912(13) 0.6125(15) 0.039(7) Uiso 0.50 1 d P
C21 C 0.0673(16) 0.2153(11) 0.5712(11) 0.017(5) Uiso 0.50 1 d PD
N1 N 0.0069(10) 0.6211(7) 0.6595(10) 0.050(4) Uani 0.50 1 d P
N2 N 0.2988(13) 0.6061(8) 0.3911(8) 0.053(4) Uani 0.50 1 d P
N3 N 0.027(2) 0.2007(8) 0.6087(15) 0.115(11) Uani 0.50 1 d PD
C1S C 0.2237(18) 0.1318(7) 0.9103(9) 0.156(9) Uani 1 1 d .
H1S1 H 0.2704 0.1042 0.8942 0.187 Uiso 1 1 calc R
H1S2 H 0.1854 0.1102 0.9427 0.187 Uiso 1 1 calc R
Cl1S Cl 0.1495(4) 0.1534(2) 0.8357(5) 0.197(3) Uani 1 1 d .
Cl2S Cl 0.2851(6) 0.1838(3) 0.9607(2) 0.215(4) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 '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
O2 C1 C3 125.4(6) . .
O2 C1 C2 116.5(5) . .
C3 C1 C2 118.1(5) . .
O1 C2 C3 126.4(6) . 5_666
O1 C2 C1 114.2(5) . .
C3 C2 C1 119.4(5) 5_666 .
C1 C3 C2 122.4(5) . 5_666
C1 C3 C19 116(2) . .
C2 C3 C19 121(2) 5_666 .
C1 C3 Cl1 117.7(5) . .
C2 C3 Cl1 119.7(5) 5_666 .
C19 C3 Cl1 3(2) . .
O3 C4 C6 125.7(5) . 5_566
O3 C4 C5 115.4(5) . .
C6 C4 C5 118.9(5) 5_566 .
O4 C5 C6 125.7(5) . .
O4 C5 C4 114.7(5) . .
C6 C5 C4 119.6(5) . .
C5 C6 C4 121.6(5) . 5_566
C5 C6 C20 120.9(14) . .
C4 C6 C20 117.6(13) 5_566 .
C5 C6 Cl2 117.6(5) . .
C4 C6 Cl2 120.8(5) 5_566 .
C20 C6 Cl2 4.4(13) . .
O5 C7 C9 125.1(5) . 7_556
O5 C7 C8 114.9(5) . .
C9 C7 C8 120.0(5) 7_556 .
O6 C8 C9 124.9(5) . .
O6 C8 C7 116.9(5) . .
C9 C8 C7 118.2(5) . .
C7 C9 C8 121.9(5) 7_556 .
C7 C9 C21 118.2(10) 7_556 .
C8 C9 C21 119.1(10) . .
C7 C9 Cl3 119.8(5) 7_556 .
C8 C9 Cl3 118.4(5) . .
C21 C9 Cl3 10.6(8) . .
O7 C10 N4 124.6(6) . .
O8 C13 N5 124.5(6) . .
O9 C16 N6 125.4(6) . .
C10 N4 C11 120.7(6) . .
C10 N4 C12 121.4(6) . .
C11 N4 C12 117.9(6) . .
C13 N5 C15 121.2(6) . .
C13 N5 C14 120.7(6) . .
C15 N5 C14 117.9(6) . .
C16 N6 C17 121.0(6) . .
C16 N6 C18 120.7(7) . .
C17 N6 C18 118.2(7) . .
C2 O1 Er1 119.9(4) . .
C1 O2 Er1 123.1(4) . .
C4 O3 Er1 122.4(4) . .
C5 O4 Er1 123.1(4) . .
C7 O5 Er1 122.8(3) . .
C8 O6 Er1 119.5(3) . .
C10 O7 Er1 146.0(5) . .
C13 O8 Er1 124.7(4) . .
C16 O9 Er1 133.9(4) . .
O7 Er1 O8 82.96(16) . .
O7 Er1 O9 75.67(15) . .
O8 Er1 O9 75.43(15) . .
O7 Er1 O5 82.78(15) . .
O8 Er1 O5 139.49(14) . .
O9 Er1 O5 135.99(14) . .
O7 Er1 O2 136.90(15) . .
O8 Er1 O2 84.88(15) . .
O9 Er1 O2 139.65(14) . .
O5 Er1 O2 80.19(14) . .
O7 Er1 O4 141.69(15) . .
O8 Er1 O4 74.18(14) . .
O9 Er1 O4 69.11(15) . .
O5 Er1 O4 133.80(13) . .
O2 Er1 O4 71.78(14) . .
O7 Er1 O3 137.11(15) . .
O8 Er1 O3 137.19(14) . .
O9 Er1 O3 97.58(15) . .
O5 Er1 O3 73.19(13) . .
O2 Er1 O3 73.59(14) . .
O4 Er1 O3 64.15(13) . .
O7 Er1 O6 70.94(15) . .
O8 Er1 O6 141.47(14) . .
O9 Er1 O6 71.03(14) . .
O5 Er1 O6 65.75(13) . .
O2 Er1 O6 133.43(14) . .
O4 Er1 O6 109.78(14) . .
O3 Er1 O6 66.93(14) . .
O7 Er1 O1 72.61(15) . .
O8 Er1 O1 72.54(15) . .
O9 Er1 O1 136.99(15) . .
O5 Er1 O1 67.03(14) . .
O2 Er1 O1 64.29(14) . .
O4 Er1 O1 126.21(14) . .
O3 Er1 O1 125.43(14) . .
O6 Er1 O1 122.63(14) . .
N2 Cl1 C3 164.6(13) . .
N1 Cl2 C6 172.0(12) . .
N3 Cl3 C9 176(2) . .
N2 C19 C3 173(5) . .
N1 C20 C6 172(3) . .
N3 C21 C9 155(3) . .
Cl2 N1 C20 7.3(19) . .
Cl1 N2 C19 8(3) . .
Cl3 N3 C21 18.3(15) . .
Cl1S C1S Cl2S 116.9(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.253(7) .
C1 C3 1.391(8) .
C1 C2 1.529(8) .
C2 O1 1.249(7) .
C2 C3 1.404(9) 5_666
C3 C2 1.404(9) 5_666
C3 C19 1.41(5) .
C3 Cl1 1.737(8) .
C4 O3 1.245(7) .
C4 C6 1.401(8) 5_566
C4 C5 1.531(8) .
C5 O4 1.249(7) .
C5 C6 1.398(8) .
C6 C4 1.401(8) 5_566
C6 C20 1.43(3) .
C6 Cl2 1.736(9) .
C7 O5 1.254(7) .
C7 C9 1.374(8) 7_556
C7 C8 1.535(7) .
C8 O6 1.240(7) .
C8 C9 1.426(8) .
C9 C7 1.374(8) 7_556
C9 C21 1.65(2) .
C9 Cl3 1.733(8) .
C10 O7 1.239(8) .
C10 N4 1.307(8) .
C11 N4 1.443(11) .
C12 N4 1.451(9) .
C13 O8 1.239(8) .
C13 N5 1.331(8) .
C14 N5 1.441(9) .
C15 N5 1.420(9) .
C16 O9 1.224(8) .
C16 N6 1.321(8) .
C17 N6 1.438(10) .
C18 N6 1.450(10) .
O1 Er1 2.500(4) .
O2 Er1 2.388(4) .
O3 Er1 2.443(4) .
O4 Er1 2.430(4) .
O5 Er1 2.381(4) .
O6 Er1 2.454(4) .
O7 Er1 2.335(4) .
O8 Er1 2.358(4) .
O9 Er1 2.380(4) .
Cl1 N2 0.813(17) .
Cl2 N1 0.772(17) .
Cl3 N3 0.84(2) .
C19 N2 1.12(4) .
C20 N1 1.08(3) .
C21 N3 0.984(18) .
C1S Cl1S 1.642(19) .
C1S Cl2S 1.643(16) .
