#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:13:03 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179562 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/31/4503167.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_4503167
loop_
_publ_author_name
'Volkringer, Christophe'
'Marrot, Jérôme'
'Férey, Gérard'
'Loiseau, Thierry'
_publ_section_title
;
 Hydrothermal Crystallization of Three Calcium-Based Hybrid Solids with
 2,6-Naphthalene- or 4,4′-Biphenyl-Dicarboxylates
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              685
_journal_paper_doi               10.1021/cg700685g
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C14 H8 Ca O7'
_chemical_formula_weight         328.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           46
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5444(3)
_cell_length_b                   30.2468(13)
_cell_length_c                   7.2194(3)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.69
_cell_volume                     1429.06(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14199
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_correction_T_min  0.8953
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0887P)²+1.9428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                1890
_reflns_number_total             2276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg700685g-file004.cif
_cod_data_source_block           wb51sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Ima2
_cod_database_code               4503167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'
'-x+1, 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
Ca Ca 0.7500 -0.02554(2) -0.0021(3) 0.0371(3) Uani 1 2 d S
O1 O 0.5836(3) 0.04753(7) 0.0685(5) 0.0459(7) Uani 1 1 d .
O2 O 0.5805(4) 0.42201(7) 0.0647(5) 0.0492(8) Uani 1 1 d .
O3 O 0.7500 -0.0512(2) 0.3150(9) 0.0746(16) Uani 1 2 d S
O4 O 0.7500 -0.08806(11) -0.2044(7) 0.0466(10) Uani 1 2 d S
O5 O 1.0000 0.0000 -0.2568(6) 0.0434(9) Uani 1 2 d S
C1 C 0.7500 0.06816(13) 0.0729(8) 0.0309(9) Uani 1 2 d S
C2 C 0.7500 0.11763(12) 0.0813(7) 0.0289(8) Uani 1 2 d S
C3 C 0.9286(6) 0.14060(11) 0.0816(11) 0.084(2) Uani 1 1 d .
H3 H 1.0523 0.1254 0.0810 0.101 Uiso 1 1 calc R
C4 C 0.9281(7) 0.18685(11) 0.0829(12) 0.092(3) Uani 1 1 d .
H4 H 1.0520 0.2019 0.0846 0.110 Uiso 1 1 calc R
C5 C 0.7500 0.21048(12) 0.0818(7) 0.0293(8) Uani 1 2 d S
C6 C 0.7500 0.25946(12) 0.0803(7) 0.0299(8) Uani 1 2 d S
C7 C 0.9260(6) 0.28298(11) 0.0789(11) 0.086(2) Uani 1 1 d .
H7 H 1.0501 0.2681 0.0817 0.103 Uiso 1 1 calc R
C8 C 0.9254(6) 0.32915(11) 0.0734(10) 0.084(2) Uani 1 1 d .
H8 H 1.0494 0.3442 0.0713 0.101 Uiso 1 1 calc R
C9 C 0.7500 0.35259(12) 0.0710(8) 0.0304(9) Uani 1 2 d S
C10 C 0.7500 0.40243(13) 0.0651(8) 0.0350(10) Uani 1 2 d S
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'
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
O1 Ca O1 138.00(14) 2_655 3
O1 Ca O4 84.73(8) 2_655 .
O1 Ca O4 84.73(8) 3 .
O1 Ca O3 72.68(10) 2_655 .
O1 Ca O3 72.68(10) 3 .
O4 Ca O3 108.9(2) . .
O1 Ca O1 127.58(10) 2_655 4_655
O1 Ca O1 78.56(9) 3 4_655
O4 Ca O1 144.98(11) . 4_655
O3 Ca O1 95.19(17) . 4_655
O1 Ca O1 78.56(9) 2_655 .
O1 Ca O1 127.58(10) 3 .
O4 Ca O1 144.98(11) . .
O3 Ca O1 95.19(17) . .
O1 Ca O1 51.30(10) 4_655 .
O1 Ca O5 69.42(9) 2_655 3_455
O1 Ca O5 146.36(13) 3 3_455
O4 Ca O5 78.53(10) . 3_455
O3 Ca O5 140.47(7) . 3_455
O1 Ca O5 98.97(8) 4_655 3_455
O1 Ca O5 66.85(9) . 3_455
O1 Ca O5 146.36(13) 2_655 .
O1 Ca O5 69.42(9) 3 .
O4 Ca O5 78.53(10) . .
O3 Ca O5 140.47(7) . .
O1 Ca O5 66.85(9) 4_655 .
O1 Ca O5 98.97(8) . .
O5 Ca O5 78.71(12) 3_455 .
O1 Ca C1 103.80(7) 2_655 .
O1 Ca C1 103.80(7) 3 .
O4 Ca C1 153.12(17) . .
O3 Ca C1 97.9(2) . .
O1 Ca C1 25.74(5) 4_655 .
O1 Ca C1 25.74(5) . .
O5 Ca C1 80.77(10) 3_455 .
O5 Ca C1 80.77(10) . .
O1 Ca Ca 43.72(5) 2_655 2_655
O1 Ca Ca 164.95(9) 3 2_655
O4 Ca Ca 109.75(3) . 2_655
O3 Ca Ca 97.88(7) . 2_655
O1 Ca Ca 90.94(6) 4_655 2_655
O1 Ca Ca 39.96(5) . 2_655
O5 Ca Ca 45.47(7) 3_455 2_655
O5 Ca Ca 116.46(4) . 2_655
C1 Ca Ca 65.21(2) . 2_655
O1 Ca Ca 164.95(9) 2_655 2_755
O1 Ca Ca 43.72(5) 3 2_755
O4 Ca Ca 109.75(3) . 2_755
O3 Ca Ca 97.88(7) . 2_755
O1 Ca Ca 39.96(5) 4_655 2_755
O1 Ca Ca 90.94(6) . 2_755
O5 Ca Ca 116.46(4) 3_455 2_755
O5 Ca Ca 45.47(7) . 2_755
C1 Ca Ca 65.21(2) . 2_755
Ca Ca Ca 129.46(4) 2_655 2_755
C1 O1 Ca 163.1(3) . 2_655
C1 O1 Ca 93.8(2) . .
Ca O1 Ca 96.32(8) 2_655 .
Ca O5 Ca 89.06(15) 2_755 .
O1 C1 O1 120.3(4) . 4_655
O1 C1 C2 119.83(18) . .
O1 C1 C2 119.84(18) 4_655 .
O1 C1 Ca 60.48(18) . .
O1 C1 Ca 60.48(18) 4_655 .
C2 C1 Ca 171.5(4) . .
C3 C2 C3 118.6(4) 4_655 .
C3 C2 C1 120.70(19) 4_655 .
C3 C2 C1 120.70(19) . .
C2 C3 C4 120.6(4) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C5 C4 C3 121.7(4) . .
C5 C4 H4 119.2 . .
C3 C4 H4 119.2 . .
C4 C5 C4 116.9(4) . 4_655
C4 C5 C6 121.53(19) . .
C4 C5 C6 121.5(2) 4_655 .
C7 C6 C7 116.6(4) 4_655 .
C7 C6 C5 121.72(19) 4_655 .
C7 C6 C5 121.72(19) . .
C6 C7 C8 121.6(3) . .
C6 C7 H7 119.2 . .
C8 C7 H7 119.2 . .
C9 C8 C7 121.8(4) . .
C9 C8 H8 119.1 . .
C7 C8 H8 119.1 . .
C8 C9 C8 116.6(4) 4_655 .
C8 C9 C10 121.7(2) 4_655 .
C8 C9 C10 121.7(2) . .
O2 C10 O2 123.8(4) 4_655 .
O2 C10 C9 118.10(18) 4_655 .
O2 C10 C9 118.11(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca O1 2.338(2) 2_655
Ca O1 2.338(2) 3
Ca O4 2.390(4) .
Ca O3 2.417(6) .
Ca O1 2.516(2) 4_655
Ca O1 2.516(2) .
Ca O5 2.580(3) 3_455
Ca O5 2.580(3) .
Ca C1 2.885(4) .
Ca Ca 3.6185(6) 2_655
Ca Ca 3.6185(6) 2_755
O1 C1 1.256(3) .
O1 Ca 2.338(2) 2_655
O2 C10 1.257(3) .
O5 Ca 2.580(3) 2_755
C1 O1 1.256(3) 4_655
C1 C2 1.497(5) .
C2 C3 1.360(4) 4_655
C2 C3 1.360(4) .
C3 C4 1.399(5) .
C3 H3 0.9300 .
C4 C5 1.367(5) .
C4 H4 0.9300 .
C5 C4 1.367(5) 4_655
C5 C6 1.482(5) .
C6 C7 1.354(4) 4_655
C6 C7 1.354(4) .
C7 C8 1.397(5) .
C7 H7 0.9300 .
C8 C9 1.349(4) .
C8 H8 0.9300 .
C9 C8 1.349(4) 4_655
C9 C10 1.508(5) .
C10 O2 1.257(3) 4_655
