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_4513536
_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         'C28 H14 Cd2 Cl12 N2 O10, C2 H6 O'
_chemical_formula_sum            'C30 H20 Cd2 Cl12 N2 O11'
_chemical_formula_weight         1234.68
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.451(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7798(12)
_cell_length_b                   12.6363(11)
_cell_length_c                   25.0522(18)
_cell_measurement_reflns_used    8763
_cell_measurement_temperature    293(2)
_cell_volume                     3971.0(6)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2003)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(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  0.0225
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19468
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+6.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                6073
_reflns_number_total             7005
_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_database_code               4513536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1Wa,H1Wb)
2.b Ternary CH refined with riding coordinates:
 C9(H9), C2(H2), C12(H12), C13(H13)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b)
2.d Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C21(H21), C24(H24), C23(H23), C20(H20), C26(H26), C27(H27)
2.e Idealised Me refined as rotating group:
 C1A(H1Aa,H1Ab,H1Ac)
2.f Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'