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_4129098
_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_absolute_configuration ad
_chemical_formula_moiety         'C72 H36 Cu O12 P4, 1(F6 P), 3(C H4 O)'
_chemical_formula_sum            'C75 H48 Cu F6 O15 P5'
_chemical_formula_weight         1521.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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            4
_cell_length_a                   13.6619(5)
_cell_length_b                   37.9460(14)
_cell_length_c                   13.6696(6)
_cell_measurement_reflns_used    9530
_cell_measurement_temperature    150
_cell_measurement_theta_max      52.041
_cell_measurement_theta_min      3.470
_cell_volume                     7086.5(5)
_computing_cell_refinement
'SAINT (2013) V8.37A; 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) V8.37A; 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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0755
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            89528
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        52.426
_diffrn_reflns_theta_max         52.426
_diffrn_reflns_theta_min         2.026
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  0.3129
_exptl_absorpt_correction_T_min  0.2271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1568 before and 0.1063 after correction. The Ratio of minimum to maximum transmission is 0.7258. 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    1.426
_exptl_crystal_description       Block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.140(9)
_refine_ls_extinction_coef       0.00057(10)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         11920
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1242P)^2^+8.7409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                10287
_reflns_number_total             11920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_010.cif
_cod_data_source_block           jw19042
_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               4129098
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.860(9)
 0.140(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C6F-O6F = C6G-O6G
 1.3 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C8C \\sim C8A \\sim C8D \\sim C8B \\sim C9A \\sim C9B \\sim C9C \\sim C9D \\sim
C10A \\sim C10C \\sim C10D \\sim C10B \\sim C11C \\sim C11D \\sim C11B \\sim
C11A \\sim C12A \\sim C12D \\sim C12B \\sim C12C: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
Uanis(P1E) \\sim Ueq, Uanis(F1E) \\sim Ueq, Uanis(F2E) \\sim Ueq, Uanis(F3E)
\\sim Ueq, Uanis(F4E) \\sim Ueq, Uanis(F5E) \\sim Ueq, Uanis(F6E) \\sim Ueq,
Uanis(P1F) \\sim Ueq, Uanis(F1F) \\sim Ueq, Uanis(F2F) \\sim Ueq, Uanis(F3F)
\\sim Ueq, Uanis(F4F) \\sim Ueq, Uanis(F5F) \\sim Ueq, Uanis(F6F) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(P1E) = Uanis(P1F)
Uanis(F1E) = Uanis(F1F)
Uanis(F2E) = Uanis(F2F)
Uanis(F3E) = Uanis(F3F)
Uanis(F4E) = Uanis(F4F)
Uanis(F5E) = Uanis(F5F)
Uanis(F6E) = Uanis(F6F)
5. Same fragment restrains
{P1E, F1E, F2E, F3E, F4E, F5E, F6E} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1F, F1F, F2F, F3F, F4F, F5F, F6F}
6. Others
 Sof(P1F)=Sof(F1F)=Sof(F2F)=Sof(F3F)=Sof(F4F)=Sof(F5F)=Sof(F6F)=1-FVAR(1)
 Sof(P1E)=Sof(F1E)=Sof(F2E)=Sof(F3E)=Sof(F4E)=Sof(F5E)=Sof(F6E)=FVAR(1)
 Sof(O1G)=Sof(H1G)=Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=0.5*(1-FVAR(3))
 Sof(O1F)=Sof(H1F)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(H1FC)=0.5*FVAR(3)
 Sof(O5G)=Sof(H5G)=Sof(C5G)=Sof(H5GA)=Sof(H5GB)=Sof(H5GC)=0.5*(1-FVAR(4))
 Sof(O5F)=Sof(H5F)=Sof(C5F)=Sof(H5FA)=Sof(H5FB)=Sof(H5FC)=0.5*FVAR(4)
 Sof(O3G)=Sof(H3G)=Sof(C3G)=Sof(H3GA)=Sof(H3GB)=Sof(H3GC)=0.5*(1-FVAR(5))
 Sof(O3F)=Sof(H3F)=Sof(C3F)=Sof(H3FA)=Sof(H3FB)=Sof(H3FC)=0.5*FVAR(5)
 Sof(O6G)=Sof(H6G)=Sof(C6G)=Sof(H6GA)=Sof(H6GB)=Sof(H6GC)=0.5*(1-FVAR(6))
 Sof(O6F)=Sof(H6F)=Sof(C6F)=Sof(H6FA)=Sof(H6FB)=Sof(H6FC)=0.5*FVAR(6)
 Fixed Sof: O2F(0.5) H2F(0.5) C2F(0.5) H2FA(0.5) H2FB(0.5) H2FC(0.5) O4F(0.5)
 H4F(0.5) C4F(0.5) H4FA(0.5) H4FB(0.5) H4FC(0.5)
7.a Riding coordinates:
 C1F(H1FA,H1FB,H1FC), C1G(H1GA,H1GB,H1GC), C2F(H2FA,H2FB,H2FC), C3F(H3FA,H3FB,
 H3FC), C3G(H3GA,H3GB,H3GC), C4F(H4FA,H4FB,H4FC), C5F(H5FA,H5FB,H5FC), C5G(H5GA,
 H5GB,H5GC), C6F(H6FA,H6FB,H6FC), C6G(H6GA,H6GB,H6GC)
7.b Aromatic/amide H refined with riding coordinates:
 C3C(H3C), C3B(H3B), C3A(H3A), C3D(H3D), C4A(H4A), C4D(H4D), C4B(H4B),
 C4C(H4C), C5D(H5D), C5A(H5A), C5B(H5B), C5C(H5C), C9A(H9A), C9B(H9B), C9C(H9C),
  C9D(H9D), C10A(H10A), C10C(H10C), C10D(H10D), C10B(H10B), C11C(H11C),
 C11D(H11D), C11B(H11B), C11A(H11A), C15A(H15A), C15B(H15B), C15D(H15D),
 C15C(H15C), C16D(H16D), C16A(H16A), C16C(H16C), C16B(H16B), C17B(H17B),
 C17A(H17A), C17C(H17C), C17D(H17D)
7.c Tetrahedral OH refined with everything fixed:
 O1F(H1F), O1G(H1G), O2F(H2F), O3F(H3F), O3G(H3G), O4F(H4F), O5F(H5F),
 O5G(H5G), O6F(H6F), O6G(H6G)
;
_shelx_res_checksum              61319
_shelx_hkl_checksum              8130
_olex2_submission_special_instructions 'No special instructions were received'