First Ferrimagnets Based on Thiocyanato-Bridges
Maliheh Mousavi; Virginie Bereau; Carine Duhayon; Philippe Guionneau; Jean-Pascal Sutter; Chem.Commun. 48 (2012) 10028–; doi:10.1039/c2cc33877g

data_7108409
_publ_section_title
;
 First Ferrimagnets Based on Thiocyanato-Bridges
;
_journal_name_full               Chem.Commun.
_journal_page_first              10028
_journal_paper_doi               10.1039/c2cc33877g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C57 H66 Mo2 N24 Ni3 S12'
_chemical_formula_sum            'C57 H66 Mo2 N24 Ni3 S12'
_chemical_formula_weight         1840.12
_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   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90.419(4)
_cell_angle_beta                 94.755(4)
_cell_angle_gamma                108.682(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5105(10)
_cell_length_b                   16.4003(13)
_cell_length_c                   19.0260(15)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     3682.9(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56578
_diffrn_reflns_theta_full        25.278
_diffrn_reflns_theta_max         28.402
_diffrn_reflns_theta_min         1.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.70
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1302
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         10632
_refine_ls_number_restraints     1039
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.0035301
_refine_ls_shift/su_mean         0.0001490
_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:
0.627 0.613 0.370
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1120
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0669
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10632
_reflns_number_total             17765
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0666
_oxford_reflns_number_all        17718
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c2cc33877g.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7108409
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
SUMFIX ELEMENT SCALES
RIDE C ( 45,X'S) H ( 452,X'S) H ( 451,X'S)
RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S)
RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 56,X'S) H ( 562,X'S) H ( 561,X'S) H ( 563,X'S)
RIDE C ( 57,X'S) H ( 572,X'S) H ( 573,X'S) H ( 571,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
SAME C(28) C(29) C(30) C(31) C(32) C(33)
CONT C(34) C(35) C(36) C(37) C(38) C(39)
CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20)
CONT AND
CONT C(280) C(290) C(300) C(310) C(320) C(330)
CONT C(340) C(350) C(360) C(370) C(380) C(390)
CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200)
REM
DELU 0.005 C(28) C(29) C(30) C(31) C(32) C(33)
CONT C(34) C(35) C(36) C(37) C(38) C(39)
CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20)
CONT AND
CONT C(280) C(290) C(300) C(310) C(320) C(330)
CONT C(340) C(350) C(360) C(370) C(380) C(390)
CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200)
REM
SIMU 0.005 C(28) C(29) C(30) C(31) C(32) C(33)
CONT C(34) C(35) C(36) C(37) C(38) C(39)
CONT C(40) C(41) C(42) N(17) N(18) N(19) N(20)
CONT AND
CONT C(280) C(290) C(300) C(310) C(320) C(330)
CONT C(340) C(350) C(360) C(370) C(380) C(390)
CONT C(400) C(410) C(420) N(170) N(180) N(190) N(200)
REM
U(IJ) 0,.001 =C(28) TO C(280) C(29) TO C(290)
CONT C(30) TO C(300) C(31) TO C(310)
CONT C(32) TO C(320) C(33) TO C(330)
CONT C(34) TO C(340) C(35) TO C(350)
CONT C(36) TO C(360) C(37) TO C(370)
CONT C(38) TO C(380) C(39) TO C(390)
CONT C(40) TO C(400) C(41) TO C(410)
CONT C(42) TO C(420)
CONT N(17) TO N(170) N(18) TO N(180)
CONT N(19) TO N(190) N(20) TO N(200)
REM
REM
SAME C(13) C(14) C(15) C(16) C(17) C(18)
CONT C(19) C(20) C(21) C(22) C(23) C(24)
CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16)
CONT AND
CONT C(130) C(140) C(150) C(160) C(170) C(180)
CONT C(190) C(200) C(210) C(220) C(230) C(240)
CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160)
REM
DELU 0.005 C(13) C(14) C(15) C(16) C(17) C(18)
CONT C(19) C(20) C(21) C(22) C(23) C(24)
CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16)
CONT AND
CONT C(130) C(140) C(150) C(160) C(170) C(180)
CONT C(190) C(200) C(210) C(220) C(230) C(240)
CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160)
REM
SIMU 0.005 C(13) C(14) C(15) C(16) C(17) C(18)
CONT C(19) C(20) C(21) C(22) C(23) C(24)
CONT C(25) C(26) C(27) N(13) N(14) N(15) N(16)
CONT AND
CONT C(130) C(140) C(150) C(160) C(170) C(180)
CONT C(190) C(200) C(210) C(220) C(230) C(240)
CONT C(250) C(260) C(270) N(130) N(140) N(150) N(160)
REM
U(IJ) 0,.001 =C(13) TO C(130) C(14) TO C(140)
CONT C(15) TO C(150) C(16) TO C(160)
CONT C(17) TO C(170) C(18) TO C(180)
CONT C(19) TO C(190) C(20) TO C(200)
CONT C(21) TO C(210) C(22) TO C(220)
CONT C(23) TO C(230) C(24) TO C(240)
CONT C(25) TO C(250) C(26) TO C(260)
CONT C(27) TO C(270)
CONT N(13) TO N(130) N(14) TO N(140)
CONT N(15) TO N(150) N(16) TO N(160)
DIST 1.45,0.02=N(23) TO C(48), C(48) TO C(49)
CONT C(49) TO C(50), C(50) TO N(24)
CONT N(23) TO C(480), C(480) TO C(490)
CONT C(490) TO C(50)
SAME N(23) C(48) C(49) C(50)
CONT AND N(23) C(480) C(490) C(50)
REM
DELU 0.005 N(23) C(48) C(49) C(50)
CONT AND N(23) C(480) C(490) C(50)
REM
SIMU 0.005 N(23) C(48) C(49) C(50)
CONT AND N(23) C(480) C(490) C(50)
REM
U(IJ) 0,.001 =C(48) TO C(480) C(49) TO C(490)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
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