#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:08:11 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190084 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/66/7226696.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_7226696
loop_
_publ_author_name
'Sun, Yuexin'
'Sun, Yayong'
'Zheng, Hao'
'Wang, Hongli'
'Han, Yi'
'Yang, Yu'
'Wang, Lei'
_publ_section_title
;
 Four calcium(ii) coordination polymers based on 2,5-dibromoterephthalic
 acid and different N-donor organic species: syntheses, structures,
 topologies, and luminescence properties
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8664
_journal_paper_doi               10.1039/C6CE01709F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.5(C80 H60 Br8 Ca2 N8 O16)'
_chemical_formula_sum            'C40 H30 Br4 Ca N4 O8'
_chemical_formula_weight         1054.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n'
_symmetry_space_group_name_Hall  '-P 2ab 2bc'
_symmetry_space_group_name_H-M   'P n n n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-07-29 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0693(5)
_cell_length_b                   12.9647(3)
_cell_length_c                   13.6267(4)
_cell_measurement_reflns_used    2386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8700
_cell_measurement_theta_min      3.6730
_cell_volume                     1955.57(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5704
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.168
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86799
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0347
_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)+(0.0331P)²+3.3151P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1392
_reflns_number_total             1736
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01709f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7226695--7226698.cif.'
_cod_database_code               7226696
_shelxl_version_number           2013-2
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, 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
Br1 Br 0.55011(6) 0.11477(3) 0.70840(3) 0.0680(2) Uani 1 1 d . . .
Ca1 Ca 0.2500 0.2500 0.2500 0.0274(3) Uani 1 4 d S T P
O1 O 0.4143(2) 0.13491(17) 0.27406(17) 0.0390(6) Uani 1 1 d . . .
N1 N 0.2089(3) 0.3474(2) 0.0778(2) 0.0352(7) Uani 1 1 d . . .
C3 C 0.5278(3) 0.1029(2) 0.5040(3) 0.0313(8) Uani 1 1 d . . .
H3 H 0.5468 0.1727 0.5080 0.038 Uiso 1 1 calc R U .
O2 O 0.6004(2) 0.1837(2) 0.3153(2) 0.0526(7) Uani 1 1 d . . .
C4 C 0.5235(3) 0.0448(2) 0.5887(2) 0.0315(7) Uani 1 1 d . . .
C1 C 0.5048(3) 0.1303(2) 0.3259(2) 0.0312(7) Uani 1 1 d . . .
C6 C 0.1694(3) 0.5096(3) -0.0015(3) 0.0404(9) Uani 1 1 d . . .
C8 C 0.2314(3) 0.3053(2) -0.0094(2) 0.0290(7) Uani 1 1 d . . .
C2 C 0.5045(3) 0.0598(2) 0.4137(2) 0.0275(7) Uani 1 1 d . . .
C7 C 0.1792(3) 0.4477(3) 0.0800(3) 0.0423(9) Uani 1 1 d . . .
H7 H 0.1642 0.4774 0.1410 0.051 Uiso 1 1 calc R U .
C9 C 0.2216(4) 0.3617(3) -0.0950(3) 0.0507(10) Uani 1 1 d . . .
H9 H 0.2357 0.3306 -0.1554 0.061 Uiso 1 1 calc R U .
C10 C 0.1905(4) 0.4648(3) -0.0901(3) 0.0514(10) Uani 1 1 d . . .
H10 H 0.1841 0.5036 -0.1473 0.062 Uiso 1 1 calc R U .
C5 C 0.1384(4) 0.6226(3) 0.0082(4) 0.0609(12) Uani 1 1 d . . .
H5A H 0.0525 0.6303 0.0147 0.091 Uiso 1 1 calc R U .
H5B H 0.1655 0.6589 -0.0491 0.091 Uiso 1 1 calc R U .
H5C H 0.1776 0.6505 0.0652 0.091 Uiso 1 1 calc R U .
H2 H 0.603(9) 0.2500 0.2500 0.15(3) Uiso 1 2 d S . P
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'
Br Br -0.2901 2.4595 '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'
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'
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 Ca1 O1 164.13(12) . 2
O1 Ca1 O1 80.05(12) 3 2
O1 Ca1 O1 102.17(11) 4 2
O1 Ca1 O1 102.17(11) . 3
O1 Ca1 O1 80.05(12) . 4
O1 Ca1 O1 164.13(12) 3 4
O1 Ca1 N1 92.56(8) 4 2
O1 Ca1 N1 122.83(8) 2 2
O1 Ca1 N1 73.48(9) 3 2
O1 Ca1 N1 72.38(8) . 2
O1 Ca1 N1 92.56(8) 2 4
O1 Ca1 N1 122.83(8) 4 4
O1 Ca1 N1 72.39(8) 3 4
O1 Ca1 N1 73.48(9) . 4
O1 Ca1 N1 92.56(8) . 3
O1 Ca1 N1 92.56(8) 3 .
O1 Ca1 N1 73.48(9) 4 .
O1 Ca1 N1 72.38(8) 2 .
O1 Ca1 N1 122.83(8) . .
O1 Ca1 N1 73.48(9) 2 3
O1 Ca1 N1 72.39(8) 4 3
O1 Ca1 N1 122.83(8) 3 3
N1 Ca1 N1 124.30(11) 2 4
N1 Ca1 N1 59.55(11) 3 4
N1 Ca1 N1 160.61(12) . 4
N1 Ca1 N1 124.30(11) . 3
N1 Ca1 N1 59.55(11) . 2
N1 Ca1 N1 160.61(12) 3 2
C1 O1 Ca1 137.3(2) . .
C8 N1 Ca1 123.50(19) . .
C8 N1 C7 117.6(3) . .
C7 N1 Ca1 118.3(2) . .
C2 C3 C4 121.3(3) . .
C3 C4 Br1 117.1(2) . .
C3 C4 C2 121.3(3) . 5_656
C2 C4 Br1 121.6(2) 5_656 .
O1 C1 O2 126.0(3) . .
O1 C1 C2 119.0(3) . .
O2 C1 C2 114.9(3) . .
C7 C6 C5 120.9(4) . .
C10 C6 C7 117.0(3) . .
C10 C6 C5 122.1(4) . .
N1 C8 C8 116.46(17) . 2
N1 C8 C9 121.5(3) . .
C9 C8 C8 122.1(2) . 2
C3 C2 C4 117.3(3) . 5_656
C3 C2 C1 117.6(3) . .
C4 C2 C1 125.0(3) 5_656 .
N1 C7 C6 124.6(3) . .
C8 C9 C10 119.4(4) . .
C6 C10 C9 119.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C4 1.889(3) .
Ca1 O1 2.375(2) 4
Ca1 O1 2.375(2) 2
Ca1 O1 2.375(2) .
Ca1 O1 2.375(2) 3
Ca1 N1 2.703(3) 2
Ca1 N1 2.703(3) 4
Ca1 N1 2.703(3) .
Ca1 N1 2.703(3) 3
O1 C1 1.227(4) .
N1 C8 1.332(4) .
N1 C7 1.341(4) .
C3 C4 1.379(4) .
C3 C2 1.376(5) .
O2 C1 1.273(4) .
C4 C2 1.392(4) 5_656
C1 C2 1.507(4) .
C6 C7 1.375(5) .
C6 C10 1.360(5) .
C6 C5 1.511(5) .
C8 C8 1.492(6) 2
C8 C9 1.381(5) .
C2 C4 1.391(4) 5_656
C9 C10 1.382(5) .
