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_4514939
_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         '2(C35 H32 O4 P), 2(C H4 O), H2 O, C10 H10 N2'
_chemical_formula_sum            'C82 H84 N2 O11 P2'
_chemical_formula_weight         1335.45
_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
_audit_creation_date             2018-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                88.647(3)
_cell_angle_beta                 83.371(3)
_cell_angle_gamma                88.178(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8783(4)
_cell_length_b                   17.6185(7)
_cell_length_c                   19.0112(7)
_cell_measurement_reflns_used    13026
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5620
_cell_measurement_theta_min      2.8920
_cell_volume                     3616.8(2)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -46.00 -21.00   1.00   60.00    --   -0.00 -82.00-150.00   25
  2  \w    -17.00  34.00   1.00   60.00    --   -0.00 -82.00-150.00   51
  3  \w     26.00  88.00   1.00   60.00    --   -0.00  19.00 -60.00   62
  4  \w    -18.00   8.00   1.00   60.00    --   -0.00 -82.00 -90.00   26
  5  \w     12.00  54.00   1.00   60.00    --   -0.00  57.00-120.00   42
  6  \w    -76.00 -17.00   1.00   60.00    --   -0.00 -77.00 120.00   59
  7  \w      2.00  32.00   1.00   60.00    --   -0.00 -77.00 120.00   30
  8  \w    -18.00  27.00   1.00   60.00    --   -0.00 -82.00  60.00   45
  9  \w     18.00  87.00   1.00   60.00    --   -0.00  38.00-150.00   69
 10  \w     -6.00  19.00   1.00   60.00    --   -0.00  38.00-120.00   25
 11  \w    -22.00   3.00   1.00   60.00    --   -0.00  57.00 -90.00   25
 12  \w    -85.00 -56.00   1.00   60.00    --   -0.00 -19.00 150.00   29
 13  \w    -49.00  19.00   1.00   60.00    --   -0.00 -27.00 -19.12   68
;
_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  0.0535
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.427
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50248
_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    1.226
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         14206
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0476P)^2^+3.4534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11791
_reflns_number_total             14206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           aj0051
_cod_database_code               4514939
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11A of O11, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H0AA of O0AA, H0AH of O0AB, H9A of O9, H7 of O7, H4 of O4
2. Restrained distances
 C44-C58 \\sim C44-C58A
 with sigma of 0.02
 C58-C59A \\sim C58A-C59B
 with sigma of 0.02
 C58-C63 \\sim C58A-C63
 with sigma of 0.02
 C59A-C60A \\sim C59B-C60B
 with sigma of 0.02
 C60A-C61 \\sim C60B-C61A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62
 with sigma of 0.02
 C44-C59A \\sim C44-C59B
 with sigma of 0.04
 C58-C60A \\sim C58A-C60B
 with sigma of 0.04
 C59A-C61 \\sim C59B-C61A
 with sigma of 0.04
 C59A-C63 \\sim C59B-C63
 with sigma of 0.04
 C60A-C62 \\sim C60B-C62
 with sigma of 0.04
 O0AA-C0AA \\sim O0AB-C0AB
 with sigma of 0.02
 O0AB-C0AB \\sim C0AA-O0AA
 with sigma of 0.02
 H1-N1 \\sim N2-H2
 with sigma of 0.02
 H2-N2 \\sim N1-H1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C58A) = Uanis(C59B) = Uanis(C60B) = Uanis(C61A)
Uanis(C0AA) = Uanis(C0AB)
Uanis(O0AA) = Uanis(O0AB)
4. Rigid body (RIGU) restrains
 O0AB, C0AB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C58, C59A, C60A, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C58A, C59B, C60B, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C0AB)=Sof(H0AE)=Sof(H0AF)=Sof(H0AG)=Sof(O0AB)=Sof(H0AH)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=FVAR(1)
 Sof(H44A)=Sof(H62A)=Sof(H63A)=Sof(C58A)=Sof(C59B)=Sof(H59B)=Sof(C60B)=
 Sof(H60B)=Sof(C61A)=Sof(H61A)=1-FVAR(2)
 Sof(H44)=Sof(C58)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61)=Sof(H61)=
 Sof(H62)=Sof(H63)=FVAR(2)
6.a Riding coordinates:
 O11(H11A)
6.b Ternary CH refined with riding coordinates:
 C7(H7A), C8(H8), C9(H9), C42(H42), C43(H43), C44(H44), C44(H44A)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38),
 C40(H40), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53),
  C54(H54), C55(H55), C59A(H59A), C60A(H60A), C61(H61), C62(H62), C62(H62A),
 C63(H63), C63(H63A), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C78(H78),
  C79(H79), C59B(H59B), C60B(H60B), C61A(H61A)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C81(H81A,H81B,H81C), C0AA(H0AB,H0AC,H0AD), C0AB(H0AE,H0AF,H0AG)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O9(H9A), O0AA(H0AA), O0AB(H0AH)
;
_shelx_res_checksum              49323
_shelx_hkl_checksum              6776
_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
;