Synthesis and crystal structures of Zn(ii) and Co(ii) coordination compounds with ortho substituted pyridine ligands: two structure types and polymorphism in the region of their coexistence
Wöhlert, Susanne; Jess, Inke; Englert, Ulli; Näther, Christian; CrystEngComm 15 (2013) 5326–; doi:10.1039/c3ce40208h

data_7209884
_publ_section_title
;
 Synthesis and crystal structures of Zn(ii) and Co(ii) coordination
 compounds with ortho substituted pyridine ligands: two structure types
 and polymorphism in the region of their coexistence
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5326
_journal_paper_doi               10.1039/c3ce40208h
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C12 H8 Br2 Co N4 S2'
_chemical_formula_sum            'C12 H8 Br2 Co N4 S2'
_chemical_formula_weight         491.09
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3517(7)
_cell_length_b                   9.6554(5)
_cell_length_c                   15.5866(8)
_cell_measurement_reflns_used    8998
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.61
_cell_volume                     1708.37(16)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Diamond (Brandenburg, 2011)
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8998
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.923
_exptl_absorpt_correction_T_max  0.6312
_exptl_absorpt_correction_T_min  0.1973
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.2095
_exptl_crystal_size_mid          0.0920
_exptl_crystal_size_min          0.0512
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0082(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0515P)^2^+4.9681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                1636
_reflns_number_total             2060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40208h.txt
_cod_data_source_block           woe1814
_cod_original_sg_symbol_H-M      'P bcn'
_cod_database_code               7209884