Structural investigations of phosphorus–nitrogen compounds. 6. Relationships between molecular parameters in per-<i>X</i>-substituted bridged spermine derivatives and basicity constants Σα<i>R</i> of substituents
Coles, Simon J; Davies, David B.; Hursthouse, Michael B.; Kiliç, Adem; Mayer, Thomas A.; Shaw, Robert A.; Yenilmez Çiftçi, Gonul; Acta Crystallographica Section B 60 (2004) 739–747; doi:10.1107/S0108768104025947

data_2102651
_publ_section_title
;
 Structural investigations of phosphorus--nitrogen compounds. 6.
 Relationships between molecular parameters in per-<i>X</i>-substituted
 bridged spermine derivatives and basicity constants \S\a<i>R</i> of
 substituents
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              739
_journal_page_last               747
_journal_paper_doi               10.1107/S0108768104025947
_journal_volume                  60
_journal_year                    2004
_chemical_formula_sum            'C42 H102 N18 P6'
_chemical_formula_weight         1045.24
_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-97
_cell_angle_alpha                111.28(3)
_cell_angle_beta                 96.87(3)
_cell_angle_gamma                93.69(3)
_cell_formula_units_Z            2
_cell_length_a                   13.476(3)
_cell_length_b                   14.437(3)
_cell_length_c                   16.340(3)
_cell_measurement_reflns_used    68138
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2921.0(13)
_computing_cell_refinement       'DENZO, COLLECT'
_computing_data_collection
'DENZO (Otwinowski, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO, COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47815
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.275
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.375
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10292
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_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.4011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                7658
_reflns_number_total             10292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5015.cif
_cod_data_source_block           2g
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2921.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2102651