Weak hydrogen bonding between acetylenic groups: the formation of diamondoid nets in the crystal structure of tetrakis(4-ethynylphenyl)methane†
Galoppini, Elena; Gilardi, Richard; Chemical Communications  (1999) 173–; doi:10.1039/a807993e

data_7110391
_publ_contact_author
;
      Richard Gilardi
      Laboratory for the Structure of Matter
      The Naval Research Laboratory, Code 6030
      Washington, D. C. ; USA 20375-5341
;
_publ_section_title
;
 Weak hydrogen bonding between acetylenic groups: the formation of
 diamondoid nets in the crystal structure of
 tetrakis(4-ethynylphenyl)methane&#x2020;
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              173
_journal_paper_doi               10.1039/a807993e
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_sum            'C43.5 H33.5'
_chemical_formula_weight         556.20
_chemical_name_systematic
;
 1,3,5,7-tetrakis(4-ethynylphenyl)adamantane/benzene [4:1] solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 121.896(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   48.460(4)
_cell_length_b                   10.5467(13)
_cell_length_c                   28.759(3)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.94
_cell_measurement_theta_min      6.17
_cell_volume                     12479(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8609
_diffrn_reflns_theta_max         45.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        4%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       thick_plate
_exptl_crystal_F_000             4712
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .11
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.000124(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_hydrogen_treatment    'riding - ideal trigonal, tetrahedral'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_obs          0.0574
_refine_ls_shift/esd_max         -0.017
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1376
_refine_ls_wR_factor_obs         0.1115
_reflns_number_observed          2985
_reflns_number_total             5051
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807993esup1.cif
_cod_data_source_block           galop02b
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] 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^)+(0.0506P)^2^+0.0000P] 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        12479.1(22)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C43.50 H33.50'
_cod_database_code               7110391