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_4129095
_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 Cu2 I2 O12 P4, C7 H8'
_chemical_formula_sum            'C79 H44 Cu2 I2 O12 P4'
_chemical_formula_weight         1689.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           84
_space_group_name_Hall           '-P 4c'
_space_group_name_H-M_alt        'P 42/m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9038(7)
_cell_length_b                   13.9038(7)
_cell_length_c                   17.3483(9)
_cell_measurement_reflns_used    9779
_cell_measurement_temperature    150
_cell_measurement_theta_max      61.077
_cell_measurement_theta_min      2.766
_cell_volume                     3353.7(3)
_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 0.997
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         61.060
_diffrn_reflns_theta_min         2.765
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    9.346
_exptl_absorpt_correction_T_max  0.2626
_exptl_absorpt_correction_T_min  0.0974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1547 before and 0.1045 after correction. The Ratio of minimum to maximum transmission is 0.3709. 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    1.673
_exptl_crystal_description       Block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.00066(11)
_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   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+1.7862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3665
_reflns_number_total             4020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_001.cif
_cod_data_source_block           jw2058
_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_original_cell_volume        3353.7(4)
_cod_database_code               4129095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.487
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1C-C7C
 1.5 with sigma of 0.002
 C2C-C7C \\sim C6C-C7C
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C1C \\sim C2C \\sim C3C \\sim C4C \\sim C5C \\sim C6C: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.002
C1C \\sim C2C \\sim C3C \\sim C4C \\sim C5C \\sim C6C \\sim C7C: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C1C) \\sim Ueq, Uanis(C2C) \\sim Ueq, Uanis(C3C) \\sim Ueq, Uanis(C4C)
\\sim Ueq, Uanis(C5C) \\sim Ueq, Uanis(C6C) \\sim Ueq, Uanis(C7C) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: C1C(0.25) C2C(0.25) H2C(0.25) C3C(0.25) H3C(0.25) C4C(0.25)
 H4C(0.25) C5C(0.25) H5C(0.25) C6C(0.25) H6C(0.25) C7C(0.25) H7CA(0.25)
 H7CB(0.25) H7CC(0.25)
5.a Me refined with riding coordinates:
 C7C(H7CA,H7CB,H7CC)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C9A(H9A),
 C9B(H9B), C10A(H10A), C10B(H10B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C),
 C6C(H6C)
5.c Fitted hexagon refined as free rotating group:
 C1C(C2C,C3C,C4C,C5C,C6C)
;
_shelx_res_checksum              38359
_shelx_hkl_checksum              36453
_olex2_submission_special_instructions 'No special instructions were received'