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_4514935
_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, C H4 O, C4 H7 N2'
_chemical_formula_sum            'C40 H43 N2 O5 P'
_chemical_formula_weight         662.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.624(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5044(3)
_cell_length_b                   23.4379(9)
_cell_length_c                   16.1485(6)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.0740
_cell_measurement_theta_min      2.9470
_cell_volume                     3496.1(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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     69.00  94.00   1.00   14.85    --    6.00  77.00   0.00   25
  2  \w     17.00  95.00   1.00   14.85    --    6.00  38.00-180.00   78
  3  \w     67.00  94.00   1.00   14.85    --    6.00  77.00 -60.00   27
  4  \w     51.00  87.00   1.00   14.85    --    6.00  77.00  90.00   36
  5  \w     56.00  84.00   1.00   14.85    --    6.00  77.00-120.00   28
  6  \w     -9.00  45.00   1.00   14.85    --    6.00 -77.00 -60.00   54
  7  \w    -59.00  23.00   1.00   14.85    --   -6.30 -82.00  30.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0632682000
_diffrn_orient_matrix_UB_12      -0.0050529000
_diffrn_orient_matrix_UB_13      0.0325738000
_diffrn_orient_matrix_UB_21      -0.0038774000
_diffrn_orient_matrix_UB_22      -0.0294469000
_diffrn_orient_matrix_UB_23      -0.0103471000
_diffrn_orient_matrix_UB_31      0.0433684000
_diffrn_orient_matrix_UB_32      0.0047360000
_diffrn_orient_matrix_UB_33      -0.0295881000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32723
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.810
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93328
_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    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.173
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0464P)^2^+1.0409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5955
_reflns_number_total             7218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           aj0050
_cod_database_code               4514935
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C120 H130 N4 O8 P1'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C9(H9)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3a), 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), N2(H2), C36(H36),
 C37(H37), C38(H38)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C40(H40a,H40b,H40c), C39(H39a,H39b,
 H39c)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5a)
;
_shelx_res_checksum              19010
_shelx_hkl_checksum              59953
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.120
_oxdiff_exptl_absorpt_empirical_full_min 0.742