Supramolecular systems built from phenylcyanamido ligands. Syntheses, crystal structures and magnetic properties
Albert Escuer; Franz A. Mautner; Núria Sanz; Ramon Vicente; Dalton Trans.  (2003) 2121–2125; doi:10.1039/b300603d

data_7012740
_publ_section_title
;
 Supramolecular systems built from phenylcyanamido ligands. Syntheses,
 crystal structures and magnetic properties
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2121
_journal_page_last               2125
_journal_paper_doi               10.1039/b300603d
_journal_year                    2003
_chemical_formula_sum            'C76 H68 Mn4 N24 O4'
_chemical_formula_weight         1601.30
_chemical_name_common            (Mn4(bipym)2(phenyl-NCN)8(MeOH)4)n
_chemical_name_systematic
; 
? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.08(3)
_cell_angle_beta                 89.47(3)
_cell_angle_gamma                86.35(3)
_cell_formula_units_Z            2
_cell_length_a                   10.931(4)
_cell_length_b                   17.269(9)
_cell_length_c                   19.955(9)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      8.9
_cell_volume                     3745(3)
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      88(2)
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       'Omega-scan; delta Omega: 1.20 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10680
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        14
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '100 min'
_diffrn_standards_number         '3  (-1 0 3; 0 0 -4; 0 -3 -2)'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         9552
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_obs          0.0788
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+15.8435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2241
_refine_ls_wR_factor_obs         0.1825
_reflns_number_observed          6171
_reflns_number_total             9562
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b300603d.txt
_cod_data_source_block           ns202a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+15.8435P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+15.8435P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3745.3(29)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012740