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_4514934
_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         'C35 H32 O4 P, C4 H7 N2'
_chemical_formula_sum            'C39 H39 N2 O4 P'
_chemical_formula_weight         630.69
_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   geom
_audit_creation_date             2018-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                93.228(7)
_cell_angle_beta                 98.981(7)
_cell_angle_gamma                109.589(9)
_cell_formula_units_Z            2
_cell_length_a                   9.6355(9)
_cell_length_b                   10.7583(10)
_cell_length_c                   17.1049(13)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      28.8920
_cell_measurement_theta_min      3.0490
_cell_volume                     1638.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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      120.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      8.00  33.00   1.00   87.63    --    1.80  56.00  78.00   25
  2  \w    -53.00 -28.00   1.00   87.63    --    1.80 -56.00 -64.00   25
  3  \w    -25.00  90.00   1.00   87.63    --    1.80  38.00  60.00  115
  4  \w    -76.00  36.00   1.00   87.63    --    1.80 -77.00-180.00  112
  5  \w    -64.00 -39.00   1.00   87.63    --    1.80 -38.00   0.00   25
  6  \w    -61.00 -16.00   1.00   87.63    --   -2.10 -82.00 120.00   45
  7  \w     -3.00  79.00   1.00   87.63    --   -2.10  19.00 -60.00   82
  8  \w    -35.00 -10.00   1.00   87.63    --   -2.10 -82.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25418
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.428
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       needle
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0675P)^2^+1.4004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4815
_reflns_number_total             6764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           aj0058
_cod_database_code               4514934
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C4-C1AA \\sim C4-C1AB
 with sigma of 0.02
 C1AA-C2AA \\sim C1AB-C2AB
 with sigma of 0.02
 C1AA-C3AA \\sim C1AB-C3AB
 with sigma of 0.02
 C4-C2AA \\sim C4-C2AB
 with sigma of 0.04
 C4-C3AA \\sim C4-C3AB
 with sigma of 0.04
 C2AA-C3AA \\sim C2AB-C3AB
 with sigma of 0.04
 C23-C24 \\sim C23-C24A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25
 with sigma of 0.02
 C24-C4AA \\sim C24A-C4AB
 with sigma of 0.02
 C26-C27 \\sim C26-C27A
 with sigma of 0.02
 C27-C0AA \\sim C27A-C0AB
 with sigma of 0.02
 C4AA-C0AA \\sim C4AB-C0AB
 with sigma of 0.02
 C23-C4AA \\sim C23-C4AB
 with sigma of 0.04
 C24-C0AA \\sim C24A-C0AB
 with sigma of 0.04
 C25-C4AA \\sim C25-C4AB
 with sigma of 0.04
 C26-C0AA \\sim C26-C0AB
 with sigma of 0.04
 C27-C4AA \\sim C27A-C4AB
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C0AB) = Uanis(C4AB) = Uanis(C24A) = Uanis(C25) = Uanis(C26)
Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C4AA) = Uanis(C0AA)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C6) = Uanis(C5)
4. Rigid body (RIGU) restrains
 C2AA, C3AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AA, C2AA, C3AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AB, C2AB, C3AB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C27, C4AA, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24A, C27A, C4AB, C0AB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C3AB)=Sof(H3AD)=Sof(H3AE)=Sof(H3AF)=Sof(C1AB)=Sof(H1AB)=Sof(C2AB)=
 Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=1-FVAR(1)
 Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3AA)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
 Sof(H23A)=Sof(H25A)=Sof(H26A)=Sof(C24A)=Sof(C4AB)=Sof(H4AB)=Sof(C0AB)=
 Sof(H0AB)=Sof(C27A)=Sof(H27A)=1-FVAR(2)
 Sof(H23)=Sof(C24)=Sof(H25)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C4AA)=Sof(H4AA)=
 Sof(C0AA)=Sof(H0AA)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C23(H23), C23(H23A), C1AA(H1AA), C1AB(H1AB)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C19(H19), C5(H5), C9(H9), C37(H37), C36(H36), C00N(H00N),
 C25(H25), C25(H25A), C18(H18), C10(H10), C15(H15), C3(H3A), C13(H13), C26(H26),
  C26(H26A), C11(H11), C17(H17), C27(H27), C31(H31), C16(H16), C12(H12),
 C33(H33), C34(H34), C32(H32), C4AA(H4AA), C0AA(H0AA), C4AB(H4AB), C0AB(H0AB),
 C27A(H27A)
6.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C3AB(H3AD,
 H3AE,H3AF), C2AB(H2AD,H2AE,H2AF)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              70604
_shelx_hkl_checksum              47743
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;