Competing ferro- and antiferromagnetic interactions in a hexagonal bipyramidal nickel thiolate cluster.
Hamaguchi, Tomohiko; Doud, Michael D.; Hilgar, Jeremy; Rinehart, Jeffrey D.; Kubiak, Clifford P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2374–2377; doi:10.1039/c5dt04861c

data_7037859
_publ_section_title
;
 Competing ferro- and antiferromagnetic interactions in a hexagonal
 bipyramidal nickel thiolate cluster.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2374
_journal_page_last               2377
_journal_paper_doi               10.1039/c5dt04861c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C72 H66 N18 Ni8 S12, 4(F6 P)'
_chemical_formula_sum            'C72 H66 F24 N18 Ni8 P4 S12'
_chemical_formula_weight         2617.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-28 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3771(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9583(3)
_cell_length_b                   22.5215(5)
_cell_length_c                   15.3686(4)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.21
_cell_volume                     4827.1(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009) and
 Yadokari-XG (Wakita, Nemoto et al., 2009)
 and ORTEP-3 for Windows (Farrugia ,1997)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009) and
Yadokari-XG (Wakita, Nemoto et al., 2009)
 and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_laue_measured_fraction_full 0.928
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39258
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.330
_diffrn_reflns_theta_min         1.717
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0449 before and 0.0349 after correction.
The Ratio of minimum to maximum transmission is 0.7511.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+9.6558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7789
_reflns_number_total             8804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04861c2.cif
_cod_data_source_block           NiCluster
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037859.cif.
;
_cod_database_code               7037859
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C2(H2), C14(H14), C25(H25), C3(H3), C20(H20), C22(H22),
 C10(H10), C13(H13), C23(H23), C8(H8), C28(H28), C5(H5), C19(H19), C15(H15),
 C24(H24), C9(H9), C7(H7), C4(H4), C18(H18), C17(H17), C12(H12), C29(H29)
2.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              17618
_olex2_submission_special_instructions 'No special instructions were received'