#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/04/1540446.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_1540446
loop_
_publ_author_name
'Banerjee, Debasis'
'Wang, Hao'
'Gong, Qihan'
'Plonka, Anna M.'
'Jagiello, Jacek'
'Wu, Haohan'
'Woerner, William R.'
'Emge, Thomas J.'
'Olson, David H.'
'Parise, John B.'
'Li, Jing'
_publ_section_title
;
 Direct structural evidence of commensurate-to-incommensurate transition
 of hydrocarbon adsorption in a microporous metal organic framework
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              759
_journal_paper_doi               10.1039/C5SC03685B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C15.31 H11.50 Ca O6 S'
_chemical_formula_sum            'C15.31 H11.5 Ca O6 S'
_chemical_formula_weight         363.5
_chemical_name_systematic
; 
 ? 
;
_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
;
2015-03-01 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6426(8)
_cell_length_b                   5.5574(4)
_cell_length_c                   22.8446(16)
_cell_measurement_temperature    100(2)
_cell_volume                     1452.50(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16471
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4365
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0324
_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)+(0.0427P)²+1.4244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                4041
_reflns_number_total             4365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc03685b2.cif
_cod_data_source_block           DB1_120B2
_cod_depositor_comments
'Adding full bibliography for 1540441--1540447.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C15.31 H11.50 Ca O6 S'
_cod_database_code               1540446
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ca1 Ca 0.63725(2) -0.25855(4) 0.221255(11) 0.00766(7) Uani 1 1 d .
S1 S 0.39739(3) -0.46701(6) 0.106089(13) 0.00781(8) Uani 1 1 d .
O1 O 0.75956(8) -0.08773(18) 0.30892(4) 0.01047(18) Uani 1 1 d .
O2 O 0.76333(9) -0.47921(18) 0.32817(4) 0.01136(19) Uani 1 1 d .
O3 O 0.51274(9) 0.47435(18) 0.25310(5) 0.01263(19) Uani 1 1 d .
O4 O 0.54161(9) 0.07891(19) 0.24366(5) 0.0134(2) Uani 1 1 d .
O5 O 0.41423(9) -0.72328(18) 0.10967(4) 0.01150(19) Uani 1 1 d .
O6 O 0.49453(8) -0.30891(19) 0.12907(4) 0.01071(18) Uani 1 1 d .
C1 C 0.77313(11) -0.2643(2) 0.34464(6) 0.0087(2) Uani 1 1 d .
C2 C 0.29730(11) -0.2903(2) -0.08989(6) 0.0084(2) Uani 1 1 d .
C3 C 0.26526(12) -0.5109(2) -0.06885(6) 0.0120(2) Uani 1 1 d .
H3 H 0.2253 -0.6263 -0.0959 0.014 Uiso 1 1 calc R
C4 C 0.29170(12) -0.5620(2) -0.00832(6) 0.0122(2) Uani 1 1 d .
H4 H 0.2690 -0.7110 0.0065 0.015 Uiso 1 1 calc R
C5 C 0.35195(11) -0.3917(2) 0.03031(6) 0.0088(2) Uani 1 1 d .
C6 C 0.38114(12) -0.1679(3) 0.01029(6) 0.0113(2) Uani 1 1 d .
H6 H 0.4196 -0.0512 0.0374 0.014 Uiso 1 1 calc R
C7 C 0.35291(12) -0.1183(2) -0.05027(6) 0.0111(2) Uani 1 1 d .
H7 H 0.3717 0.0342 -0.0647 0.013 Uiso 1 1 calc R
C8 C 0.28003(11) -0.3932(2) 0.14147(6) 0.0089(2) Uani 1 1 d .
C9 C 0.19084(12) -0.5614(2) 0.14017(6) 0.0116(2) Uani 1 1 d .
H9 H 0.1912 -0.7073 0.1185 0.014 Uiso 1 1 calc R
C10 C 0.10135(12) -0.5121(2) 0.17107(6) 0.0115(2) Uani 1 1 d .
H10 H 0.0410 -0.6267 0.1715 0.014 Uiso 1 1 calc R
C11 C 0.10016(11) -0.2948(2) 0.20137(6) 0.0092(2) Uani 1 1 d .
C12 C 0.49323(11) 0.2567(2) 0.26234(6) 0.0096(2) Uani 1 1 d .
C13 C 0.18832(11) -0.1257(2) 0.20036(6) 0.0099(2) Uani 1 1 d .
H13 H 0.1857 0.0243 0.2200 0.012 Uiso 1 1 calc R
C14 C 0.28006(11) -0.1745(2) 0.17088(6) 0.0100(2) Uani 1 1 d .
H14 H 0.3411 -0.0612 0.1709 0.012 Uiso 1 1 calc R
C1P C -0.0205(4) -0.0254(10) 0.04959(18) 0.0858(17) Uani 0.874(9) 1 d PD
H1P1 H -0.0687 0.0537 0.0748 0.129 Uiso 0.874(9) 1 calc PR
H1P2 H 0.0616 -0.0222 0.0696 0.129 Uiso 0.874(9) 1 calc PR
H1P3 H -0.0460 -0.1926 0.0425 0.129 Uiso 0.874(9) 1 calc PR
C2P C -0.0316(5) 0.0876(18) -0.0010(4) 0.080(3) Uani 0.437(4) 1 d PD
H2P1 H -0.0071 0.2554 0.0091 0.096 Uiso 0.437(4) 1 calc PR
H2P2 H -0.1166 0.0938 -0.0169 0.096 Uiso 0.437(4) 1 calc PR
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
O3 Ca1 O4 95.60(4) 1_545 .
O3 Ca1 O2 168.81(4) 1_545 2_655
O4 Ca1 O2 82.49(4) . 2_655
O3 Ca1 O1 88.67(4) 1_545 2_645
O4 Ca1 O1 174.96(4) . 2_645
O2 Ca1 O1 92.81(4) 2_655 2_645
O3 Ca1 O1 107.54(4) 1_545 .
O4 Ca1 O1 74.33(4) . .
O2 Ca1 O1 82.64(4) 2_655 .
O1 Ca1 O1 106.96(2) 2_645 .
O3 Ca1 O6 80.21(4) 1_545 .
O4 Ca1 O6 90.31(4) . .
O2 Ca1 O6 88.76(4) 2_655 .
O1 Ca1 O6 87.78(3) 2_645 .
O1 Ca1 O6 163.21(4) . .
O3 Ca1 O2 72.98(3) 1_545 .
O4 Ca1 O2 110.61(3) . .
O2 Ca1 O2 118.05(2) 2_655 .
O1 Ca1 O2 73.18(3) 2_645 .
O1 Ca1 O2 48.51(3) . .
O6 Ca1 O2 147.14(3) . .
O3 Ca1 C1 87.05(4) 1_545 .
O4 Ca1 C1 89.55(4) . .
O2 Ca1 C1 103.92(4) 2_655 .
O1 Ca1 C1 93.35(3) 2_645 .
O1 Ca1 C1 24.68(3) . .
O6 Ca1 C1 167.19(4) . .
O2 Ca1 C1 24.66(3) . .
O3 Ca1 Ca1 81.75(3) 1_545 2_645
O4 Ca1 Ca1 146.96(3) . 2_645
O2 Ca1 Ca1 105.86(3) 2_655 2_645
O1 Ca1 Ca1 36.38(2) 2_645 2_645
O1 Ca1 Ca1 75.16(3) . 2_645
O6 Ca1 Ca1 121.24(3) . 2_645
O2 Ca1 Ca1 37.03(2) . 2_645
C1 Ca1 Ca1 57.48(3) . 2_645
O3 Ca1 Ca1 141.85(3) 1_545 2_655
O4 Ca1 Ca1 70.37(3) . 2_655
O2 Ca1 Ca1 47.64(3) 2_655 2_655
O1 Ca1 Ca1 107.74(3) 2_645 2_655
O1 Ca1 Ca1 35.26(2) . 2_655
O6 Ca1 Ca1 133.05(3) . 2_655
O2 Ca1 Ca1 79.13(2) . 2_655
C1 Ca1 Ca1 58.52(3) . 2_655
Ca1 Ca1 Ca1 91.450(12) 2_645 2_655
O5 S1 O6 119.35(6) . .
O5 S1 C8 108.30(6) . .
O6 S1 C8 108.19(6) . .
O5 S1 C5 107.68(6) . .
O6 S1 C5 106.45(6) . .
C8 S1 C5 106.15(6) . .
C1 O1 Ca1 141.14(9) . 2_655
C1 O1 Ca1 102.29(8) . .
Ca1 O1 Ca1 108.36(4) 2_655 .
C1 O2 Ca1 138.63(9) . 2_645
C1 O2 Ca1 81.51(8) . .
Ca1 O2 Ca1 95.33(3) 2_645 .
C12 O3 Ca1 145.50(9) . 1_565
C12 O4 Ca1 173.13(10) . .
S1 O6 Ca1 137.77(6) . .
O2 C1 O1 123.50(12) . .
O2 C1 C2 118.85(12) . 4_656
O1 C1 C2 117.60(12) . 4_656
O2 C1 Ca1 73.84(7) . .
O1 C1 Ca1 53.04(7) . .
C2 C1 Ca1 155.99(9) 4_656 .
C7 C2 C3 120.16(12) . .
C7 C2 C1 119.23(12) . 4
C3 C2 C1 120.61(12) . 4
C4 C3 C2 119.97(12) . .
C3 C4 C5 118.99(12) . .
C6 C5 C4 121.70(12) . .
C6 C5 S1 119.24(10) . .
C4 C5 S1 119.01(10) . .
C7 C6 C5 118.57(12) . .
C6 C7 C2 120.50(12) . .
C14 C8 C9 122.07(12) . .
C14 C8 S1 119.70(10) . .
C9 C8 S1 118.22(10) . .
C10 C9 C8 118.87(12) . .
C9 C10 C11 120.04(12) . .
C10 C11 C13 120.04(12) . .
C10 C11 C12 120.72(12) . 2_545
C13 C11 C12 119.19(12) . 2_545
O4 C12 O3 126.63(13) . .
O4 C12 C11 116.91(12) . 2
O3 C12 C11 116.45(12) . 2
C14 C13 C11 120.67(12) . .
C8 C14 C13 118.26(12) . .
C1P C2P C1P 126.7(7) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O3 2.2858(10) 1_545
Ca1 O4 2.2870(10) .
Ca1 O2 2.3472(10) 2_655
Ca1 O1 2.3605(10) 2_645
Ca1 O1 2.4254(10) .
Ca1 O6 2.4448(10) .
Ca1 O2 2.8802(11) .
Ca1 C1 2.9658(13) .
Ca1 Ca1 3.8809(4) 2_645
Ca1 Ca1 3.8809(4) 2_655
S1 O5 1.4379(10) .
S1 O6 1.4514(10) .
S1 C8 1.7600(13) .
S1 C5 1.7641(13) .
O1 C1 1.2672(16) .
O1 Ca1 2.3605(10) 2_655
O2 C1 1.2511(16) .
O2 Ca1 2.3472(10) 2_645
O3 C12 1.2557(16) .
O3 Ca1 2.2858(10) 1_565
O4 C12 1.2509(17) .
C1 C2 1.5007(18) 4_656
C2 C7 1.3908(18) .
C2 C3 1.3926(18) .
C2 C1 1.5007(18) 4
C3 C4 1.3892(18) .
C4 C5 1.3919(18) .
C5 C6 1.3891(18) .
C6 C7 1.3891(18) .
C8 C14 1.3888(18) .
C8 C9 1.3934(18) .
C9 C10 1.3898(18) .
C10 C11 1.3935(18) .
C11 C13 1.3949(18) .
C11 C12 1.5119(18) 2_545
C12 C11 1.5118(18) 2
C13 C14 1.3910(18) .
C1P C2P 1.301(10) .
C2P C1P 1.402(9) 3
