Substantial exchange coupling for {Mo-NCS-M} combination: illustration for 1-D [{Mo(NCS)6}{NiL}2(NCS)]n.
Mousavi, Maliheh; Béreau, Virgine; Desplanches, Cédric; Duhayon, Carine; Sutter, Jean-Pascal; Chemical communications (Cambridge, England) 46 (2010) 7519–7521; doi:10.1039/c0cc02498h

data_7113064
_publ_section_title
;
 Substantial exchange coupling for {Mo-NCS-M} combination: illustration
 for 1-D [{Mo(NCS)6}{NiL}2(NCS)]n.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7519
_journal_page_last               7521
_journal_paper_doi               10.1039/c0cc02498h
_journal_volume                  46
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H44 Mo N15 Ni2 S7, C2 H3 N'
_chemical_formula_sum            'C39 H47 Mo N16 Ni2 S7'
_chemical_formula_weight         1177.73
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 108.947(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3601(4)
_cell_length_b                   23.0402(8)
_cell_length_c                   10.9979(5)
_cell_measurement_reflns_used    11008
_cell_measurement_temperature    180
_cell_measurement_theta_max      32
_cell_measurement_theta_min      3
_cell_volume                     2482.95(18)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_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    'Sir2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_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  0.062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27227
_diffrn_reflns_theta_full        29.777
_diffrn_reflns_theta_max         32.366
_diffrn_reflns_theta_min         2.638
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.96
_refine_ls_abs_structure_details 'Flack (1983), 2939 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.13(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000591
_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:
2.74 -1.49 1.84
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0667
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0460
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              -34
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                8235
_reflns_number_total             11466
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0500
_oxford_reflns_number_all        11440
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c0cc02498h.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C39 H47 Mo1 N16 Ni2 S7'
_cod_database_code               7113064