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_2102650
_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 H54 N18 P6'
_chemical_formula_weight         996.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.599(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.586(10)
_cell_length_b                   9.660(2)
_cell_length_c                   18.449(5)
_cell_measurement_reflns_used    38071
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.91
_cell_volume                     5433(3)
_computing_cell_refinement       'DENZO  & COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO  & COLLECT'
_computing_molecular_graphics    'PLATON (Spek 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.544
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f & \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  0.1294
_diffrn_reflns_av_sigmaI/netI    0.1976
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10652
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_correction_T_min  0.9435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      2.105
_refine_ls_R_factor_all          0.2388
_refine_ls_R_factor_gt           0.1174
_refine_ls_shift/su_max          0.254
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+22.2230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2772
_reflns_number_gt                2316
_reflns_number_total             5213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5015.cif
_cod_data_source_block           2f
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2_1/c
_cod_database_code               2102650
_cod_database_fobs_code          2102650