Building Large Structures with Curved Aromatic Surfaces by Complexing Metals with Phosphangulene.
Heskia, Alice; Maris, Thierry; Aguiar, Pedro M.; Wuest, James D.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b08179

data_4129097
_publ_section_title
;
 Building Large Structures with Curved Aromatic Surfaces by Complexing
 Metals with Phosphangulene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b08179
_journal_year                    2019
_chemical_formula_moiety         'C72 H36 Cu O12 P4, B F4'
_chemical_formula_sum            'C72 H36 B Cu F4 O12 P4'
_chemical_formula_weight         1367.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.119(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0917(2)
_cell_length_b                   14.0561(3)
_cell_length_c                   34.6177(7)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.718
_cell_measurement_theta_min      2.957
_cell_volume                     5824.7(2)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            82853
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.687
_diffrn_reflns_theta_min         2.243
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.162
_exptl_absorpt_correction_T_max  0.1217
_exptl_absorpt_correction_T_min  0.0392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1050 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.3221. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       Block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00214(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+9.3790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12351
_reflns_number_total             13385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_006.cif
_cod_data_source_block           jw1905
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4129097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.684
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B1-F1A \\sim B1-F2A \\sim B1-F3A \\sim B1-F4A \\sim B1-F1B \\sim B1-F2B \\sim
B1-F3B \\sim B1-F4B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
F1A \\sim F2A \\sim F3A \\sim F4A \\sim F1B \\sim F2B \\sim F3B \\sim F4B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Same fragment restrains
{F1A, F2A, F3A, F4A} sigma for 1-2: 0.02, 1-3: 0.04
as
{F1B, F2B, F3B, F4B}
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3D(H3D), C3B(H3B), C3C(H3C), C4A(H4A), C4B(H4B), C4D(H4D),
 C4C(H4C), C5C(H5C), C5B(H5B), C5A(H5A), C5D(H5D), C9A(H9A), C9D(H9D), C9B(H9B),
  C9C(H9C), C10C(H10C), C10B(H10B), C10A(H10A), C10D(H10D), C11B(H11B),
 C11D(H11D), C11C(H11C), C11A(H11A), C15C(H15C), C15B(H15B), C15D(H15D),
 C15A(H15A), C16D(H16D), C16B(H16B), C16A(H16A), C16C(H16C), C17B(H17B),
 C17D(H17D), C17A(H17A), C17C(H17C)
;
_shelx_res_checksum              52899
_shelx_hkl_checksum              77082
_olex2_submission_special_instructions 'No special instructions were received'