Exceptional sensitivity to the synthetic approach and halogen substituent for Zn(ii) coordination assemblies with 5-halonicotinic acids.
Li, Cheng-Peng; Chen, Jing; Mu, Yu-Hai; Du, Miao; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11109–11118; doi:10.1039/c5dt00420a

data_7034981
_publ_section_title
;
 Exceptional sensitivity to the synthetic approach and halogen substituent
 for Zn(ii) coordination assemblies with 5-halonicotinic acids.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11109
_journal_page_last               11118
_journal_paper_doi               10.1039/c5dt00420a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H6 Br2 N2 O4 Zn, 0.8(H2 O), 0.35(H2 O)'
_chemical_formula_sum            'C12 H8.3 Br2 N2 O5.15 Zn'
_chemical_formula_weight         488.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-04-27 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.944(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.782(5)
_cell_length_b                   7.787(5)
_cell_length_c                   26.565(17)
_cell_measurement_reflns_used    2354
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.62
_cell_volume                     1598.0(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.941
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            8192
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.402
_diffrn_reflns_theta_min         1.544
_exptl_absorpt_coefficient_mu    6.561
_exptl_absorpt_correction_T_max  0.4394
_exptl_absorpt_correction_T_min  0.3847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1213 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.5537.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            COLORLESS
_exptl_crystal_colour_primary    COLORLESS
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.1101
_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/[\s^2^(Fo^2^)+(0.0374P)^2^+32.1083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2614
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00420a2.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7034975--7034981.cif.
;
_cod_original_formula_sum        'C12 H8.30 Br2 N2 O5.15 Zn'
_cod_database_code               7034981
_shelx_estimated_absorpt_t_max   0.440
_shelx_estimated_absorpt_t_min   0.385
_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. Restrained distances
 O5-H5A = O5-H5B
 0.85 with sigma of 0.01
3. Others
 Fixed Sof: O5(0.8) H5A(0.8) H5B(0.8) O6(0.35)
4.a Riding coordinates:
 O5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'