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_4129096
_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         'C54 H27 Cl2 Cu2 O9 P3'
_chemical_formula_sum            'C54 H27 Cl2 Cu2 O9 P3'
_chemical_formula_weight         1110.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                105.882(2)
_cell_angle_beta                 105.468(2)
_cell_angle_gamma                105.195(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8679(4)
_cell_length_b                   13.9505(5)
_cell_length_c                   17.0453(6)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    150
_cell_measurement_theta_max      58.367
_cell_measurement_theta_min      2.519
_cell_volume                     2233.61(15)
_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 0.985
_diffrn_measured_fraction_theta_max 0.971
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51082
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         58.745
_diffrn_reflns_theta_min         2.518
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    6.891
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.5462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1470 before and 0.0698 after correction. The Ratio of minimum to maximum transmission is 0.7268. 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    1.651
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00071(7)
_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   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     909
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0117P)^2^+4.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7897
_reflns_number_total             9402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_011.cif
_cod_data_source_block           jw1914
_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        2233.61(14)
_cod_database_code               4129096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.278
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
P1A \\sim O1A \\sim O2A \\sim O3A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim
C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A
\\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim P1D
\\sim O1D \\sim O2D \\sim O3D \\sim C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D
\\sim C6D \\sim C7D \\sim C8D \\sim C9D \\sim C10D \\sim C11D \\sim C12D \\sim
C13D \\sim C14D \\sim C15D \\sim C16D \\sim C17D \\sim C18D: within 2A with
sigma of 0.055 and sigma for terminal atoms of 0.11
Uanis(P1A) = Uanis(P1D)
Uanis(O1A) = Uanis(O1D)
Uanis(O2A) = Uanis(O2D)
Uanis(O3A) = Uanis(O3D)
Uanis(C1A) = Uanis(C1D)
Uanis(C2A) = Uanis(C2D)
Uanis(C3A) = Uanis(C3D)
Uanis(C4A) = Uanis(C4D)
Uanis(C5A) = Uanis(C5D)
Uanis(C6A) = Uanis(C6D)
Uanis(C7A) = Uanis(C7D)
Uanis(C8A) = Uanis(C8D)
Uanis(C9A) = Uanis(C9D)
Uanis(C10A) = Uanis(C10D)
Uanis(C11A) = Uanis(C11D)
Uanis(C12A) = Uanis(C12D)
Uanis(C13A) = Uanis(C13D)
Uanis(C14A) = Uanis(C14D)
Uanis(C15A) = Uanis(C15D)
Uanis(C16A) = Uanis(C16D)
Uanis(C17A) = Uanis(C17D)
Uanis(C18A) = Uanis(C18D)
3. Same fragment restrains
{P1A, O1A, O2A, O3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A,
C12A, C13A, C14A, C15A, C16A, C17A, C18A} sigma for 1-2: 0.001, 1-3: 0.04
as
{P1D, O1D, O2D, O3D, C1D, C2D, C3D, C4D, C5D, C6D, C7D, C8D, C9D, C10D, C11D,
C12D, C13D, C14D, C15D, C16D, C17D, C18D}
4. Others
 Sof(P1D)=Sof(O1D)=Sof(O2D)=Sof(O3D)=Sof(C1D)=Sof(C2D)=Sof(C3D)=Sof(H3D)=
 Sof(C4D)=Sof(H4D)=Sof(C5D)=Sof(H5D)=Sof(C6D)=Sof(C7D)=Sof(C8D)=Sof(C9D)=
 Sof(H9D)=Sof(C10D)=Sof(H10D)=Sof(C11D)=Sof(H11D)=Sof(C12D)=Sof(C13D)=Sof(C14D)=
 Sof(C15D)=Sof(H15D)=Sof(C16D)=Sof(H16D)=Sof(C17D)=Sof(H17D)=Sof(C18D)=1-FVAR(1)
 Sof(P1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=
 Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C3C(H3C), C4C(H4C), C4B(H4B), C5C(H5C), C5B(H5B), C9C(H9C),
 C9B(H9B), C10B(H10B), C10C(H10C), C11B(H11B), C11C(H11C), C15B(H15B),
 C15C(H15C), C16B(H16B), C16C(H16C), C17C(H17C), C17B(H17B), C3A(H3A), C4A(H4A),
  C5A(H5A), C9A(H9A), C10A(H10A), C11A(H11A), C15A(H15A), C16A(H16A),
 C17A(H17A), C3D(H3D), C4D(H4D), C5D(H5D), C9D(H9D), C10D(H10D), C11D(H11D),
 C15D(H15D), C16D(H16D), C17D(H17D)
;
_shelx_res_checksum              22064
_shelx_hkl_checksum              15283
_olex2_submission_special_instructions 'No special instructions were received'