#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:30:03 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179532 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/01/4500151.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_4500151
loop_
_publ_author_name
'Liang, Po-Ching'
'Liu, Hsin-Kuan'
'Yeh, Chun-Ting'
'Lin, Chia-Her'
'Zima, Vítězslav'
_publ_section_title
;
 Supramolecular Assembly of Calcium Metal−Organic Frameworks with
 Structural Transformations
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              699
_journal_paper_doi               10.1021/cg101114h
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C8 H8 Ca O8'
_chemical_formula_sum            'C8 H8 Ca O8'
_chemical_formula_weight         272.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.367(2)
_cell_angle_beta                 93.316(2)
_cell_angle_gamma                91.769(2)
_cell_formula_units_Z            2
_cell_length_a                   6.0146(2)
_cell_length_b                   7.6214(3)
_cell_length_c                   11.0855(5)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.363
_cell_measurement_theta_min      2.762
_cell_volume                     490.90(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2010)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8239
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.7991
_exptl_absorpt_correction_T_min  0.7751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0250
_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)+(0.0401P)²+0.1594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                2312
_reflns_number_total             2414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101114h_si_007.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4500151
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
_atom_site_refinement_flags
Ca1 Ca 0.13601(4) 0.07262(3) 0.66779(2) 0.01777(9) Uani 1 1 d .
O1 O 0.52515(14) 0.10292(12) 0.64047(9) 0.02247(19) Uani 1 1 d .
O2 O 0.17432(14) -0.11911(12) 0.46405(8) 0.02010(18) Uani 1 1 d .
O3 O -0.68549(17) 0.83469(13) 1.04276(10) 0.0293(2) Uani 1 1 d .
H1 H -0.7846 0.8406 1.0912 0.035 Uiso 1 1 calc R
O4 O -0.06221(18) 0.55058(14) 0.78990(10) 0.0325(2) Uani 1 1 d .
O5 O -0.04567(15) 0.27702(12) 0.82532(9) 0.0246(2) Uani 1 1 d .
O6 O 0.24572(16) 0.37268(12) 0.66204(9) 0.0276(2) Uani 1 1 d .
H2 H 0.1638 0.4519 0.6953 0.033 Uiso 1 1 calc R
O7 O -0.14271(17) -0.13582(15) 0.70858(11) 0.0369(3) Uani 1 1 d .
H3 H -0.2697 -0.1145 0.6874 0.055 Uiso 1 1 d R
H4 H -0.1434 -0.2278 0.7343 0.055 Uiso 1 1 d R
O8 O 0.31863(19) -0.05240(16) 0.81830(10) 0.0373(3) Uani 1 1 d .
H5 H 0.2699 -0.0967 0.8722 0.056 Uiso 1 1 d R
H6 H 0.4324 0.0014 0.8555 0.056 Uiso 1 1 d R
C1 C 0.63975(18) 0.17759(15) 0.57550(10) 0.0170(2) Uani 1 1 d .
C2 C 0.31278(19) 0.58710(16) 0.54302(11) 0.0192(2) Uani 1 1 d .
H7 H 0.1855 0.6453 0.5720 0.023 Uiso 1 1 calc R
C3 C 0.37199(19) 0.43517(15) 0.58230(11) 0.0182(2) Uani 1 1 d .
C4 C 0.56258(18) 0.34419(15) 0.53856(11) 0.0170(2) Uani 1 1 d .
C5 C -0.4171(2) 0.63426(17) 0.94797(12) 0.0236(3) Uani 1 1 d .
H8 H -0.3617 0.7249 0.9136 0.028 Uiso 1 1 calc R
C6 C -0.3191(2) 0.46750(17) 0.92433(11) 0.0202(2) Uani 1 1 d .
C7 C -0.5964(2) 0.66708(17) 1.02228(11) 0.0217(2) Uani 1 1 d .
C8 C -0.12922(19) 0.43157(16) 0.84103(11) 0.0205(2) 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'
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'
Ca Ca 0.2262 0.3064 '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'
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
O8 Ca1 O5 90.96(4) . .
O8 Ca1 O6 118.15(4) . .
O5 Ca1 O6 72.08(3) . .
O8 Ca1 O1 74.18(4) . .
O5 Ca1 O1 122.74(3) . .
O6 Ca1 O1 68.11(3) . .
O8 Ca1 O2 155.17(4) . 2_556
O5 Ca1 O2 83.45(3) . 2_556
O6 Ca1 O2 83.14(3) . 2_556
O1 Ca1 O2 128.78(3) . 2_556
O8 Ca1 O2 109.43(4) . .
O5 Ca1 O2 155.88(3) . .
O6 Ca1 O2 107.24(3) . .
O1 Ca1 O2 76.66(3) . .
O2 Ca1 O2 72.63(3) 2_556 .
O8 Ca1 O7 76.46(4) . .
O5 Ca1 O7 81.11(4) . .
O6 Ca1 O7 149.13(3) . .
O1 Ca1 O7 141.94(3) . .
O2 Ca1 O7 78.78(3) 2_556 .
O2 Ca1 O7 91.01(4) . .
O8 Ca1 Ca1 140.31(3) . 2_556
O5 Ca1 Ca1 119.72(3) . 2_556
O6 Ca1 Ca1 96.30(3) . 2_556
O1 Ca1 Ca1 104.21(2) . 2_556
O2 Ca1 Ca1 36.33(2) 2_556 2_556
O2 Ca1 Ca1 36.31(2) . 2_556
O7 Ca1 Ca1 83.70(3) . 2_556
C1 O1 Ca1 135.12(8) . .
C1 O2 Ca1 124.20(7) 2_656 2_556
C1 O2 Ca1 123.67(8) 2_656 .
Ca1 O2 Ca1 107.37(3) 2_556 .
C7 O3 H1 109.5 . .
C8 O5 Ca1 137.77(8) . .
C3 O6 Ca1 131.18(7) . .
C3 O6 H2 109.5 . .
Ca1 O6 H2 115.5 . .
Ca1 O7 H3 113.0 . .
Ca1 O7 H4 136.4 . .
H3 O7 H4 110.4 . .
Ca1 O8 H5 131.2 . .
Ca1 O8 H6 117.5 . .
H5 O8 H6 100.7 . .
O1 C1 O2 123.07(10) . 2_656
O1 C1 C4 120.77(10) . .
O2 C1 C4 116.16(10) 2_656 .
C3 C2 C4 122.23(10) . 2_666
C3 C2 H7 118.9 . .
C4 C2 H7 118.9 2_666 .
O6 C3 C2 120.33(10) . .
O6 C3 C4 119.91(10) . .
C2 C3 C4 119.75(10) . .
C2 C4 C3 118.02(10) 2_666 .
C2 C4 C1 118.35(10) 2_666 .
C3 C4 C1 123.63(10) . .
C7 C5 C6 120.75(11) . .
C7 C5 H8 119.6 . .
C6 C5 H8 119.6 . .
C5 C6 C7 118.85(10) . 2_467
C5 C6 C8 120.36(11) . .
C7 C6 C8 120.78(11) 2_467 .
O3 C7 C5 118.08(11) . .
O3 C7 C6 121.52(10) . 2_467
C5 C7 C6 120.40(11) . 2_467
O4 C8 O5 123.28(10) . .
O4 C8 C6 119.90(10) . .
O5 C8 C6 116.82(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O8 2.3537(10) .
Ca1 O5 2.3762(9) .
Ca1 O6 2.3776(9) .
Ca1 O1 2.3888(9) .
Ca1 O2 2.3932(9) 2_556
Ca1 O2 2.3943(9) .
Ca1 O7 2.4122(10) .
O1 C1 1.2467(14) .
O2 C1 1.2774(13) 2_656
O2 Ca1 2.3933(9) 2_556
O3 C7 1.3721(14) .
O3 H1 0.8200 .
O4 C8 1.2511(15) .
O5 C8 1.2709(15) .
O6 C3 1.3599(13) .
O6 H2 0.8200 .
O7 H3 0.8193 .
O7 H4 0.8200 .
O8 H5 0.8192 .
O8 H6 0.8197 .
C1 O2 1.2775(13) 2_656
C1 C4 1.5059(15) .
C2 C3 1.3838(16) .
C2 C4 1.3941(15) 2_666
C2 H7 0.9300 .
C3 C4 1.4059(15) .
C4 C2 1.3940(15) 2_666
C5 C7 1.3864(16) .
C5 C6 1.3894(17) .
C5 H8 0.9300 .
C6 C7 1.4016(17) 2_467
C6 C8 1.4991(15) .
C7 C6 1.4016(17) 2_467
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H1 O5 0.82 1.78 2.5069(13) 146.9 2_467
O6 H2 O4 0.82 1.83 2.6044(12) 156.9 .
O7 H3 O1 0.82 2.24 2.9331(13) 142.6 1_455
O7 H4 O4 0.82 2.00 2.8017(14) 165.4 1_545
O8 H5 O3 0.82 2.09 2.8285(14) 150.2 1_645
O8 H6 O3 0.82 2.03 2.8472(16) 171.6 2_567
