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_4330998
_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         'C25.50 H26 N8 O4.50 Zn2'
_chemical_formula_sum            'C25.5 H26 N8 O4.5 Zn2'
_chemical_formula_weight         647.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                94.286(7)
_cell_angle_beta                 98.378(7)
_cell_angle_gamma                106.098(8)
_cell_formula_units_Z            2
_cell_length_a                   8.9636(7)
_cell_length_b                   11.8050(11)
_cell_length_c                   13.7543(12)
_cell_measurement_reflns_used    7684
_cell_measurement_temperature    110
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1373.2(2)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED, (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      110
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.883
_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  0.048
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23918
_diffrn_reflns_theta_full        26.662
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         3.403
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.73
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0763
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.0003712
_refine_ls_shift/su_mean         0.0000148
_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: 
 15.0 10.2 12.8 5.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0854
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5409
_reflns_number_total             6840
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      0.16
_oxford_refine_ls_r_factor_ref   0.0551
_oxford_refine_ls_scale          2.593(6)
_oxford_reflns_number_all        6829
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3012958_si_002_2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C25.50 H26 N8 O4.50 Zn2'
_cod_database_code               4330998
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;