ABAB Homoleptic Bis(phthalocyaninato)lanthanide(III) Complexes: Original Octupolar Design Leading to Giant Quadratic Hyperpolarizability.
Ayhan, Mehmet Menaf; Singh, Anu; Jeanneau, Erwann; Ahsen, Vefa; Zyss, Joseph; Ledoux-Rak, Isabelle; Gürek, Ayşe Gül; Hirel, Catherine; Bretonnière, Yann; Andraud, Chantal; Inorganic chemistry 53 (2014) 4359–4370; doi:10.1021/ic4031188

data_4337953
_publ_section_title
;
 ABAB Homoleptic Bis(phthalocyaninato)lanthanide(III) Complexes: Original
 Octupolar Design Leading to Giant Quadratic Hyperpolarizability.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4359
_journal_page_last               4370
_journal_paper_doi               10.1021/ic4031188
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C112 H128 N16 Nd S8, 2(C H Cl3)'
_chemical_formula_sum            'C114 H130 Cl6 N16 Nd S8'
_chemical_formula_weight         2337.88
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                   23.2750(10)
_cell_length_b                   29.4040(10)
_cell_length_c                   32.015(2)
_cell_measurement_reflns_used    11735
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5236
_cell_measurement_theta_min      3.3651
_cell_volume                     21910.4(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            46611
_diffrn_reflns_theta_full        26.667
_diffrn_reflns_theta_max         29.587
_diffrn_reflns_theta_min         3.372
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9728
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_min          0.301
_refine_diff_density_max         4.50
_refine_diff_density_min         -4.49
_refine_ls_extinction_coef       715.121
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.0056201
_refine_ls_shift/su_mean         0.0002538
_refine_ls_structure_factor_coef Fsqd
_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: 
 589. 909. 434. 97.7 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2057
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2057
_reflns_limit_h_max              31
_reflns_limit_h_min              0
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                5947
_reflns_number_total             6932
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      37.40
_oxford_refine_ls_r_factor_ref   0.1007
_oxford_refine_ls_scale          0.2496(3)
_oxford_reflns_number_all        6931
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic4031188_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4337951--4337954.cif.'
_cod_original_sg_symbol_H-M      'F d d d '
_cod_original_formula_sum        'C114 H130 Cl6 N16 Nd1 S8'
_cod_database_code               4337953
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 233,X'S) H   ( 234,X'S)  H   ( 231,X'S) H   ( 232,X'S)
 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 343,X'S) H   ( 344,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) H   ( 423,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
U(IJ)'S  0.0, 0.010000 = C(33) TO C(34) 
U(IJ)'S  0.0, 0.010000 = C(34) TO C(35) 
U(IJ)'S  0.0, 0.010000 = C(35) TO C(37) 
U(IJ)'S  0.0, 0.010000 = C(37) TO C(40) 
U(IJ)'S  0.0, 0.010000 = C(40) TO C(41) 
U(IJ)'S  0.0, 0.010000 = C(34) TO C(36) 
U(IJ)'S  0.0, 0.010000 = C(36) TO C(38) 
U(IJ)'S  0.0, 0.010000 = C(38) TO C(39) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(42) 
DISTANCE 1.550000 , 0.010000 = C(34) TO C(35) 
DISTANCE 1.550000 , 0.010000 = C(34) TO C(36) 
DISTANCE 1.550000 , 0.010000 = C(34) TO C(36) 
DISTANCE 1.550000 , 0.010000 = C(35) TO C(37) 
DISTANCE 1.550000 , 0.010000 = C(37) TO C(40) 
DISTANCE 1.550000 , 0.010000 = C(40) TO C(41) 
DISTANCE 1.550000 , 0.010000 = C(36) TO C(38) 
DISTANCE 1.550000 , 0.010000 = C(38) TO C(39) 
DISTANCE 1.550000 , 0.010000 = C(39) TO C(42) 
U(IJ)'S  0.0, 0.010000 = C(22) TO C(23) 
U(IJ)'S  0.0, 0.010000 = C(23) TO C(26) 
U(IJ)'S  0.0, 0.010000 = C(26) TO C(25) 
U(IJ)'S  0.0, 0.010000 = C(25) TO C(28) 
U(IJ)'S  0.0, 0.010000 = C(23) TO C(24) 
U(IJ)'S  0.0, 0.010000 = C(24) TO C(27) 
U(IJ)'S  0.0, 0.010000 = C(27) TO C(29) 
DISTANCE 1.550000 , 0.010000 = C(23) TO C(24) 
DISTANCE 1.550000 , 0.010000 = C(24) TO C(27) 
DISTANCE 1.550000 , 0.010000 = C(27) TO C(29) 
DISTANCE 1.550000 , 0.010000 = C(23) TO C(26) 
DISTANCE 1.550000 , 0.010000 = C(26) TO C(25) 
DISTANCE 1.550000 , 0.010000 = C(25) TO C(28) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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