Series of Dicyanamide-Interlaced Assembly of Zinc-Schiff-Base Complexes: Crystal Structure and Photophysical and Thermal Studies
Monami Maiti; Dipali Sadhukhan; Santarupa Thakurta; Syamantak Roy; Guillaume Pilet; Ray J. Butcher; Aline Nonat; Loïc J. Charbonnière; Samiran Mitra; Inorganic Chemistry 51 (2012) 12176–12187; doi:10.1021/ic3012958

data_4330997
_publ_section_title
;
 Series of Dicyanamide-Interlaced Assembly of Zinc-Schiff-Base Complexes:
 Crystal Structure and Photophysical and Thermal Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12176
_journal_page_last               12187
_journal_paper_doi               10.1021/ic3012958
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C19 H14 Cl2 N5 O2 Zn1.50'
_chemical_formula_sum            'C19 H14 Cl2 N5 O2 Zn1.5'
_chemical_formula_weight         513.33
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.058(5)
_cell_length_b                   8.565(5)
_cell_length_c                   21.175(5)
_cell_measurement_reflns_used    7974
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     4001(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17965
_diffrn_reflns_theta_full        25.206
_diffrn_reflns_theta_max         29.310
_diffrn_reflns_theta_min         1.846
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.12
_refine_diff_density_min         -1.01
_refine_ls_extinction_coef       11(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.0012234
_refine_ls_shift/su_mean         0.0000332
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 6.18 1.10 4.03 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0513
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0482
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3940
_reflns_number_total             4720
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      0.36
_oxford_refine_ls_r_factor_ref   0.0414
_oxford_refine_ls_scale          1.790(4)
_oxford_reflns_number_all        4704
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3012958_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C19 H14 Cl2 N5 O2 Zn1.50'
_cod_database_code               4330997
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.300000 , 0.002000 = N(43) TO C(46) 
DISTANCE 1.300000 , 0.002000 = N(43) TO C(44) 
DISTANCE 1.200000 , 0.020000 = C(46) TO N(47) 
U(IJ)'S  0.0, 0.010000 = C(44) TO N(45) 
U(IJ)'S  0.0, 0.010000 = C(44) TO N(43) 
U(IJ)'S  0.0, 0.010000 = C(42) TO N(43) 
U(IJ)'S  0.0, 0.010000 = C(46) TO N(43) 
U(IJ)'S  0.0, 0.010000 = C(46) TO N(47) 
END                                                                             
;