Synthesis of Borophosphonate Cage Compounds: Influence of Substituent and Concentration Effects on Product Distribution in Condensation Reactions of Aryl Phosphonic Acids and Boronic Acids
Liu, Qian; Contrella, Nathan D.; Filatov, Alexander S.; Jordan, Richard F.; Organometallics 34 (2015) 254–; doi:10.1021/om501101q

data_4085031
_publ_section_title
;
 Synthesis of Borophosphonate Cage Compounds: Influence of Substituent and
 Concentration Effects on Product Distribution in Condensation Reactions
 of Aryl Phosphonic Acids and Boronic Acids
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              254
_journal_paper_doi               10.1021/om501101q
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C84 H104 B4 O16 P4'
_chemical_formula_sum            'C84 H104 B4 O16 P4'
_chemical_formula_weight         1536.79
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9467(13)
_cell_length_b                   13.9467(13)
_cell_length_c                   29.586(3)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.48
_cell_volume                     5754.8(10)
_computing_cell_refinement       'SAINT V.8.34 (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 v.2014.7-1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V.8.34 (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'APEX2 v.2014.7-1 (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 v.2014.7-1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-08 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-08 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            77112
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.9577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2012/1 (Bruker AXS Inc.)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
;
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5123
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+10.1121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                4858
_reflns_number_total             5123
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om501101q_si_003.cif
_cod_data_source_block           3d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085030--4085032.cif.
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_cod_original_cell_volume        5754.8(12)
_cod_database_code               4085031