#------------------------------------------------------------------------------
#$Date: 2019-11-08 04:31:13 +0200 (Fri, 08 Nov 2019) $
#$Revision: 225370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/27/1552773.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_1552773
loop_
_publ_author_name
'MENG, Gaoxiang'
'LI, Qiang'
'YANG, Yongming'
_publ_section_title
;
 Crystal Structure of
 Catena-((μ₈-benzene-1,2,4,5-tetracarboxylato)-triaqua-calcium(II)-copper(II))
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              49
_journal_paper_doi               10.2116/xraystruct.35.49
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         'C10 H8 Ca Cu O11'
_chemical_formula_sum            'C10 H8 Ca Cu O11'
_chemical_formula_weight         407.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-15
_cell_angle_alpha                90
_cell_angle_beta                 126.365(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1365(13)
_cell_length_b                   13.2077(12)
_cell_length_c                   8.8865(8)
_cell_measurement_reflns_used    1863
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.76
_cell_volume                     1336.1(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003) '
_computing_data_collection       ' Bruker APEX2'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5798
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.362
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1185
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0779
_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)+65.0050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1082
_reflns_number_total             1185
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            35_49_1.txt
_cod_data_source_block           I
_cod_database_code               1552773
_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   0.960
_shelx_estimated_absorpt_t_min   0.903
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.60513(12) 0.7500 0.0154(4) Uani 1 2 d S T P
Ca1 Ca 0.5000 0.90501(19) 0.7500 0.0181(6) Uani 1 2 d S T P
O1 O 0.4090(5) 0.6203(5) 0.8579(9) 0.0277(15) Uani 1 1 d . . .
O2 O 0.3960(7) 0.7781(5) 0.7727(12) 0.042(2) Uani 1 1 d . . .
O3 O 0.3919(6) 0.9791(5) 1.2753(10) 0.0338(17) Uani 1 1 d . . .
O4 O 0.3553(6) 0.8780(6) 1.4329(9) 0.042(2) Uani 1 1 d . . .
O5 O 0.3527(7) 0.6070(9) 0.4947(12) 0.070(3) Uani 1 1 d . . .
H5A H 0.3250 0.6589 0.4327 0.105 Uiso 1 1 d R . .
H5B H 0.3465 0.5588 0.4236 0.105 Uiso 1 1 d R . .
O6 O 0.5000 0.4350(10) 0.7500 0.085(5) Uani 1 2 d S T P
H6 H 0.4796 0.4105 0.8113 0.127 Uiso 1 1 d R . .
C1 C 0.3039(7) 0.7304(6) 0.9129(11) 0.0143(17) Uani 1 1 d . . .
C2 C 0.3437(7) 0.8080(7) 1.0431(12) 0.0191(18) Uani 1 1 d . . .
H2 H 0.4076 0.8487 1.0706 0.023 Uiso 1 1 calc R . .
C3 C 0.2927(6) 0.8278(6) 1.1343(11) 0.0132(16) Uani 1 1 d . . .
C4 C 0.3724(7) 0.7086(7) 0.8371(11) 0.0174(18) Uani 1 1 d . U .
C5 C 0.3499(7) 0.9011(8) 1.2919(12) 0.024(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'
H H 0.0000 0.0000 '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'
Cu Cu 0.3201 1.2651 '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'
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 Cu1 O1 168.6(4) 2_656 .
O1 Cu1 O6 95.70(19) . .
O1 Cu1 O6 95.70(19) 2_656 .
O5 Cu1 O1 89.3(3) 2_656 .
O5 Cu1 O1 90.5(3) . .
O5 Cu1 O1 89.3(3) . 2_656
O5 Cu1 O1 90.5(3) 2_656 2_656
O5 Cu1 O5 178.6(7) 2_656 .
O5 Cu1 O6 90.7(4) 2_656 .
O5 Cu1 O6 90.7(4) . .
O2 Ca1 O2 87.3(4) 2_656 .
O2 Ca1 O4 86.0(3) 2_656 1_554
O2 Ca1 O4 86.0(3) . 2_657
O2 Ca1 O4 81.2(3) 2_656 2_657
O2 Ca1 O4 81.2(3) . 1_554
O3 Ca1 O2 176.1(3) 5_677 .
O3 Ca1 O2 88.8(2) 6_575 .
O3 Ca1 O2 176.1(3) 6_575 2_656
O3 Ca1 O2 88.8(2) 5_677 2_656
O3 Ca1 O3 95.0(4) 5_677 6_575
O3 Ca1 O4 93.7(3) 6_575 1_554
O3 Ca1 O4 98.3(3) 6_575 2_657
O3 Ca1 O4 93.7(3) 5_677 2_657
O3 Ca1 O4 98.3(3) 5_677 1_554
O4 Ca1 O4 162.3(4) 1_554 2_657
C4 O1 Cu1 110.4(5) . .
C4 O2 Ca1 160.7(7) . .
C5 O3 Ca1 166.1(6) . 5_677
C5 O4 Ca1 131.7(6) . 1_556
Cu1 O5 H5A 122.8 . .
Cu1 O5 H5B 114.4 . .
H5A O5 H5B 108.9 . .
Cu1 O6 H6 113.3 . .
C2 C1 C3 119.9(7) . 7_567
C2 C1 C4 117.7(7) . .
C3 C1 C4 122.4(7) 7_567 .
C1 C2 H2 119.1 . .
C1 C2 C3 121.9(7) . .
C3 C2 H2 119.1 . .
C1 C3 C5 122.1(7) 7_567 .
C2 C3 C1 118.2(8) . 7_567
C2 C3 C5 119.3(7) . .
O1 C4 C1 115.8(7) . .
O2 C4 O1 124.5(8) . .
O2 C4 C1 119.5(8) . .
O3 C5 O4 125.0(9) . .
O3 C5 C3 117.4(8) . .
O4 C5 C3 117.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.019(6) 2_656
Cu1 O1 2.019(5) .
Cu1 O5 1.970(8) .
Cu1 O5 1.970(8) 2_656
Cu1 O6 2.248(13) .
Ca1 O2 2.317(7) .
Ca1 O2 2.317(7) 2_656
Ca1 O3 2.267(7) 5_677
Ca1 O3 2.267(7) 6_575
Ca1 O4 2.328(7) 2_657
Ca1 O4 2.328(7) 1_554
O1 C4 1.244(11) .
O2 C4 1.227(10) .
O3 Ca1 2.267(7) 5_677
O3 C5 1.240(12) .
O4 Ca1 2.328(7) 1_556
O4 C5 1.247(11) .
O5 H5A 0.8193 .
O5 H5B 0.8639 .
O6 H6 0.8191 .
C1 C2 1.390(12) .
C1 C3 1.397(11) 7_567
C1 C4 1.500(10) .
C2 H2 0.9500 .
C2 C3 1.393(11) .
C3 C1 1.397(11) 7_567
C3 C5 1.486(12) .
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
O5 H5A O2 0.82 2.65 3.225(13) 128.6 7_566
O5 H5B O1 0.86 2.71 3.503(13) 153.8 6_565
O6 H6 O1 0.82 2.41 3.002(7) 130.2 5_667
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu1 O1 C4 O2 -5.0(11) . .
Cu1 O1 C4 C1 -179.5(5) . .
Ca1 O2 C4 O1 -75(2) . .
Ca1 O2 C4 C1 99.6(19) . .
Ca1 O3 C5 O4 109(3) 5_677 .
Ca1 O3 C5 C3 -68(3) 5_677 .
Ca1 O4 C5 O3 -34.4(15) 1_556 .
Ca1 O4 C5 C3 143.2(7) 1_556 .
C1 C2 C3 C1 -2.3(13) . 7_567
C1 C2 C3 C5 170.9(8) . .
C1 C3 C5 O3 -146.6(8) 7_567 .
C1 C3 C5 O4 35.6(12) 7_567 .
C2 C1 C4 O1 123.2(9) . .
C2 C1 C4 O2 -51.5(12) . .
C2 C3 C5 O3 40.5(12) . .
C2 C3 C5 O4 -137.3(9) . .
C3 C1 C2 C3 2.3(14) 7_567 .
C3 C1 C4 O1 -52.9(11) 7_567 .
C3 C1 C4 O2 132.3(9) 7_567 .
C4 C1 C2 C3 -173.9(8) . .
