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_4514941
_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         'C82 H92 Mg N4 O12 P2'
_chemical_formula_sum            'C82 H92 Mg N4 O12 P2'
_chemical_formula_weight         1411.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.698(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.4738(6)
_cell_length_b                   10.2253(2)
_cell_length_c                   25.1238(4)
_cell_measurement_reflns_used    12337
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      70.4520
_cell_measurement_theta_min      4.5380
_cell_volume                     8420.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega    2.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 64

  2 omega   46.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   37.0000  -30.0000 76

  3 omega   86.00  164.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -30.0000 78

  4 omega   81.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  120.0000 26

  5 omega   41.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 72

  6 omega   66.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 26

  7 omega   76.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 25

  8 omega   65.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -120.0000 52

  9 omega   53.00  118.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -119.0000 -101.0000 65

 10 omega   64.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 45

 11 omega   64.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   90.0000 28

 12 omega   46.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   60.0000 26

 13 omega   38.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   60.0000 55

 14 omega   54.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000    0.0000 31

 15 omega   42.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -30.0000 37

 16 omega   43.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 52

 17 omega   49.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 26

 18 omega   42.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 30

 19 omega   41.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000  -60.0000 134

 20 omega   92.00  118.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  156.0000  139.0000 26

 21 omega   25.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 92

 22 omega   35.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 27

 23 omega   36.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  150.0000 55

 24 omega   36.00  146.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000   60.0000 110

 25 omega   38.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000    0.0000 57

 26 omega    1.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  120.0000 95

 27 omega  -19.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 49

 28 omega  -41.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  119.0000  -16.0000 27

 29 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -37.0000  150.0000 44

 30 omega  -65.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0239936000
_diffrn_orient_matrix_UB_12      0.0017783000
_diffrn_orient_matrix_UB_13      -0.0592145000
_diffrn_orient_matrix_UB_21      0.0400057000
_diffrn_orient_matrix_UB_22      0.0226455000
_diffrn_orient_matrix_UB_23      -0.0200523000
_diffrn_orient_matrix_UB_31      0.0058017000
_diffrn_orient_matrix_UB_32      -0.1489525000
_diffrn_orient_matrix_UB_33      -0.0037377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28475
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.337
_diffrn_reflns_theta_min         3.593
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00051(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8111
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+5.7712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7188
_reflns_number_total             8111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           tifrh013
_cod_database_code               4514941
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.802
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2-O2
 0.85 with sigma of 0.002
 P1-H2
 2.1 with sigma of 0.004
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C23(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              53445
_shelx_hkl_checksum              74111
_shelx_fab_checksum              1931
_olex2_submission_special_instructions 'No special instructions were received'