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_4331000
_publ_section_title
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 Series of Dicyanamide-Interlaced Assembly of Zinc-Schiff-Base Complexes:
 Crystal Structure and Photophysical and Thermal Studies
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_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_absolute_configuration ad
_chemical_formula_moiety         'C152 H112 Br16 N40 O16 Zn12'
_chemical_formula_sum            'C152 H112 Br16 N40 O16 Zn12'
_chemical_formula_weight         4817.84
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.349(5)
_cell_length_b                   27.916(5)
_cell_length_c                   18.025(5)
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     16278(6)
_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      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.844
_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  0.081
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13843
_diffrn_reflns_theta_full        26.134
_diffrn_reflns_theta_max         29.698
_diffrn_reflns_theta_min         3.424
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.737
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_description       plate
_exptl_crystal_F_000             9408
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.20
_refine_diff_density_min         -1.47
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   1.009(18)
_refine_ls_extinction_coef       12(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0408
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.0006138
_refine_ls_shift/su_mean         0.0000160
_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: 
 2.19 0.834 0.770 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1230
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0640
_reflns_limit_h_max              44
_reflns_limit_h_min              0
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -22
_reflns_number_gt                5436
_reflns_number_total             8196
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      94.85
_oxford_refine_ls_r_factor_ref   0.0567
_oxford_refine_ls_scale          0.0943(2)
_oxford_reflns_number_all        8182
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ic3012958_si_002_4.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_database_code               4331000
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
CONT ENANTIO 
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) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 412,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
EQUIV C(15,U'S) UNTIL C(16) 
EQUIV C(32,U'S) UNTIL C(33) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
U(IJ)'S  0.0, 0.010000 = N(40) TO C(41) 
U(IJ)'S  0.0, 0.010000 = N(71) TO C(72) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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