Structural Diversity in Supramolecular Organization of Anionic Phosphate Monoesters: Role of Cations.
Santra, Biswajit; Mandal, Debdeep; Gupta, Vivek; Kalita, Pankaj; Kumar, Vierandra; Narayanan, Ramakirushnan Suriya; Dey, Atanu; Chrysochos, Nicolas; Mohammad, Akbar; Singh, Ajeet; Zimmer, Michael; Dalapati, Rana; Biswas, Shyam; Schulzke, Carola; Chandrasekhar, Vadapalli; Scheschkewitz, David; Jana, Anukul; ACS omega 4 (2019) 2118–2133; doi:10.1021/acsomega.8b03192

data_4514938
_publ_section_title
;
 Structural Diversity in Supramolecular Organization of Anionic Phosphate
 Monoesters: Role of Cations.
;
_journal_issue                   1
_journal_name_full               'ACS omega'
_journal_page_first              2118
_journal_page_last               2133
_journal_paper_doi               10.1021/acsomega.8b03192
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety
'C33 H28 O4 P, C6 H13 N2, C H4 O, C1.8 H3.4 N O0.5, H2 O, C0.6 O0.5, 0.6(C)'
_chemical_formula_sum            'C43 H50.4 N3 O7 P'
_chemical_formula_weight         752.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                94.548(5)
_cell_angle_beta                 104.485(5)
_cell_angle_gamma                111.120(5)
_cell_formula_units_Z            2
_cell_length_a                   9.510(5)
_cell_length_b                   13.081(5)
_cell_length_c                   17.645(5)
_cell_measurement_reflns_used    5068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.34
_cell_volume                     1947.3(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1346
_diffrn_reflns_av_unetI/netI     0.1860
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_min         2.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1626 before and 0.0825 after correction. The Ratio of minimum to maximum transmission is 0.7766. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       needle
_exptl_crystal_F_000             801
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.2243
_refine_ls_R_factor_gt           0.1144
_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^)+(0.1410P)^2^+8.6678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2617
_refine_ls_wR_factor_ref         0.3317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4122
_reflns_number_total             8060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           24apra
_cod_original_formula_sum        'C43 H50.40 N3 O7 P'
_cod_database_code               4514938
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4 of O4, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H7 of O7, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O5A) \\sim
Ueq, Uanis(C102) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.0002
Uanis(C103) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(P1) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.0002
Uanis(P1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0002
3. Others
 Fixed Sof: O5A(0.5) O5B(0.5) C103(0.6) C102(0.4) H10a(0.4) H10b(0.4)
 H10c(0.4) C1A(0.6) C1B(0.4) H1Ba(0.4) H1Bb(0.4) H1Bc(0.4)
4.a Free rotating group:
 O15(H15a,H15b)
4.b Ternary CH refined with riding coordinates:
 N2(H2), C8(H8), C21(H21)
4.c Secondary CH2 refined with riding coordinates:
 C37(H37a,H37b), C39(H39a,H39b), C36(H36a,H36b), C38(H38a,H38b), C35(H35a,
 H35b), C34(H34a,H34b)
4.d Me refined with riding coordinates:
 C7(H7a,H7b,H7c)
4.e Aromatic/amide H refined with riding coordinates:
 C27(H27), C23(H23), C5(H5), C19(H19), C26(H26), C10(H10), C3(H3), C29(H29),
 C13(H13), C18(H18), C14(H14), C30(H30), C33(H33), C20(H20), C17(H17), C24(H24),
  C16(H16), C25(H25), C11(H11), C12(H12), C31(H31), C32(H32), C1AA(H1AA)
4.f Idealised Me refined as rotating group:
 C50(H50a,H50b,H50c), C102(H10a,H10b,H10c), C1B(H1Ba,H1Bb,H1Bc)
4.g Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7)
;
_shelx_res_checksum              53749
_shelx_hkl_checksum              94840
_olex2_submission_special_instructions 'No special instructions were received'