On the Reliability of C−H···O Interactions in Crystal Engineering: Synthesis and Structure of Two Hydrogen Bonded Phosphonium Bis(aryloxide) Salts
Broder, Charlotte K.; Davidson, Matthew G.; Forsyth, V. Trevor; Howard, Judith A. K.; Lamb, Sarah; Mason, Sax A.; Crystal Growth & Design 2 (2002) 163–; doi:10.1021/cg025503q

data_4505795
_publ_section_title
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 On the Reliability of C&#x2212;H&#x00B7;&#x00B7;&#x00B7;O Interactions in
 Crystal Engineering:&#x2009; Synthesis and Structure of Two Hydrogen
 Bonded Phosphonium Bis(aryloxide) Salts
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_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              163
_journal_paper_doi               10.1021/cg025503q
_journal_volume                  2
_journal_year                    2002
_chemical_formula_sum            'C73 H88 N2 O2 P2'
_chemical_formula_weight         1087.39
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8957(2)
_cell_length_b                   18.6462(2)
_cell_length_c                   18.9466(2)
_cell_measurement_reflns_used    6497
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      51.5
_cell_measurement_theta_min      2.825
_cell_volume                     6322.23(12)
_computing_cell_refinement       'ILL program Rafd19'
_computing_data_collection       'ILL programs HKLgen and Mad'
_computing_data_reduction        'ILL program Retreat'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.826
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'D19 at ILL'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Nuclear reactor'
_diffrn_radiation_wavelength     1.30990
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17603
_diffrn_reflns_theta_full        59.46
_diffrn_reflns_theta_max         59.46
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  0.6182
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   D19abs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             787
_exptl_crystal_size_max          3.85
_exptl_crystal_size_mid          2.70
_exptl_crystal_size_min          2.60
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+67.0792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                6468
_reflns_number_total             6777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg025503q_s1.cif
_cod_data_source_block           1b:CH3CN_Neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'Refall' changed
to 'refall' 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 

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_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4505795