Syntheses, Crystal Structures, and Properties of Four Metal‒Organic Complexes Based on 1,4,5,6,7,7-Hexachlorobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic Acid
Yang, Jie; Liu, Xiaobin; Wang, Xiaoqing; Dai, Fangna; Zhou, Yan; Dong, Bin; Zhang, Liangliang; Liu, Yanru; Sun, Daofeng; Crystal Growth & Design 15 (2015) 4198–; doi:10.1021/acs.cgd.5b00164

data_4513535
_publ_section_title
;
 Syntheses, Crystal Structures, and Properties of Four Metal--Organic
 Complexes Based on
 1,4,5,6,7,7-Hexachlorobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic Acid
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4198
_journal_paper_doi               10.1021/acs.cgd.5b00164
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C33 H18 Cl12 Cu2 N3 O9'
_chemical_formula_sum            'C33 H18 Cl12 Cu2 N3 O9'
_chemical_formula_weight         1152.98
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.765(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.316(3)
_cell_length_b                   13.288(3)
_cell_length_c                   29.130(6)
_cell_measurement_reflns_used    2741
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.34
_cell_volume                     4457.6(18)
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21998
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0588
_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/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                4728
_reflns_number_total             7856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00164_si_002.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 4513533--4513536.cif.'
_cod_original_cell_volume        4457.6(17)
_cod_database_code               4513535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB)
2.b Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C12(H12), C11(H11)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C30(H30), C29(H29), C28(H28), C23(H23), C26(H26),
 C25(H25), C22(H22), C27(H27), C19(H19), C20(H20)
;