Preparation of a 'twisted basket'Mn4N8 cluster: a two-hydrogen-atom reduced analogue of the Mn4N8 pinned butterfly
Michael R. Gau; Clifton R. Hamilton; Michael J. Zdilla; Chem.Commun. 50 (2014) 7780–; doi:10.1039/C4CC02872D

data_7115273
_publ_section_title
;
 Preparation of a 'twisted basket'Mn4N8 cluster: a two-hydrogen-atom
 reduced analogue of the Mn4N8 pinned butterfly
;
_journal_name_full               Chem.Commun.
_journal_page_first              7780
_journal_paper_doi               10.1039/C4CC02872D
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         '[C48 H44 Mn4 N8] . [C5 H5 N]4'
_chemical_formula_sum            'C88 H84 Mn4 N16'
_chemical_formula_weight         1585.47
_chemical_melting_point          ?
_chemical_name_common            'Twisted Basket Mn4'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1979(16)
_cell_length_b                   22.599(2)
_cell_length_c                   40.496(5)
_cell_measurement_reflns_used    4341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.41
_cell_measurement_theta_min      2.454
_cell_volume                     16654(3)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX2 Report Generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.582
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       'Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.582
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            11276
_diffrn_reflns_point_group_measured_fraction_full 0.487
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.820
_diffrn_reflns_theta_min         1.522
_diffrn_source                   'Fine-focused Sealed Tube'
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   11723 Corrected reflections written to file mo_1713_0m.hkl
 Estimated minimum and maximum transmission:  0.6669  0.7446
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             6592
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
This structure exhibits heavy disorder amongst several of the rings     
(pyridine and phenyl) and the lattice solvent. The lattice solvent was  
unmodelable, and treated with SQUEEZE. The electron cout from SQUEEZE   
was 1362, almost identical to two pyridine solvent molecules per        
asymmetric unit (theory 1344). 
;
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 1116 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.030(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         3678
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+2.1930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_full    0.390
_reflns_Friedel_fraction_max     0.672
_reflns_number_gt                3182
_reflns_number_total             3678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02872d2.cif
_cod_data_source_block           squeeze
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7115273
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.909
_shelxl_version_number           2013-3
_shelx_res_checksum              91673