Four calcium(ii) coordination polymers based on 2,5-dibromoterephthalic acid and different N-donor organic species: syntheses, structures, topologies, and luminescence properties
Sun, Yuexin; Sun, Yayong; Zheng, Hao; Wang, Hongli; Han, Yi; Yang, Yu; Wang, Lei; CrystEngComm 18 (2016) 8664–; doi:10.1039/C6CE01709F

data_7226697
_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         'C32 H16 Br8 Ca3 O20, C12 H12 N4, 2(H2 O)'
_chemical_formula_sum            'C44 H32 Br8 Ca3 N4 O22'
_chemical_formula_weight         1728.25
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                74.417(5)
_cell_angle_beta                 84.716(5)
_cell_angle_gamma                83.300(5)
_cell_formula_units_Z            1
_cell_length_a                   10.0545(6)
_cell_length_b                   11.5943(6)
_cell_length_c                   12.4010(7)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9990
_cell_measurement_theta_min      2.7240
_cell_volume                     1380.21(14)
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5095
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0296653000
_diffrn_orient_matrix_UB_12      0.0346896000
_diffrn_orient_matrix_UB_13      -0.0506579000
_diffrn_orient_matrix_UB_21      0.0631222000
_diffrn_orient_matrix_UB_22      -0.0327271000
_diffrn_orient_matrix_UB_23      0.0131891000
_diffrn_orient_matrix_UB_31      -0.0141896000
_diffrn_orient_matrix_UB_32      -0.0423871000
_diffrn_orient_matrix_UB_33      -0.0282851000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9646
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.3190P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4001
_reflns_number_total             4844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01709f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7226695--7226698.cif.'
_cod_original_cell_volume        1380.20(13)
_cod_database_code               7226697
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 N1 O1 Zn1'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1
 0.86 with sigma of 0.01
3.a Free rotating group:
 O11(H11A,H11B)
3.b Rotating group:
 O9(H9A), O10(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C21(H21), C18(H18), C11(H11), C22(H22), C8(H8), C19(H19),
 C17(H17)
;
_shelx_res_checksum              6694