Oligomeric phosphate clusters in macrocyclic channels
Bowman-James, Kristin; Pramanik, Subhamay; Day, Victor W.; Thordarson, Pall; CrystEngComm  (2022) –; doi:10.1039/D2CE00756H

data_7245486
_publ_section_title
;
 Oligomeric phosphate clusters in macrocyclic channels
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00756H
_journal_year                    2022
_chemical_formula_moiety
'C36 H51 N12 O6, H O4 P, H2 O4 P, 3(H3 O4 P), 2(H2 O)'
_chemical_formula_sum            'C36 H67 N12 O28 P5'
_chemical_formula_weight         1270.86
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                70.4003(10)
_cell_angle_beta                 73.1350(11)
_cell_angle_gamma                69.4031(11)
_cell_formula_units_Z            2
_cell_length_a                   14.1582(2)
_cell_length_b                   14.7759(3)
_cell_length_c                   14.9206(3)
_cell_measurement_reflns_used    5699
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.59
_cell_measurement_theta_min      5.18
_cell_volume                     2699.64(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24062
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.381
_diffrn_reflns_theta_min         5.177
_diffrn_source                   'Bruker MicroStar microfocus rotating anode'
_exptl_absorpt_coefficient_mu    2.465
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         9422
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0598P)^2^+0.6502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6852
_reflns_number_total             9422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00756h2.cif
_cod_data_source_block           kbjq84h
_cod_database_code               7245486
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              24270
_shelx_hkl_checksum              28712