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_4514940
_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         'C80 H88 Mg N4 O12 P2, 2(C3 H7 N O)'
_chemical_formula_sum            'C86 H102 Mg N6 O14 P2'
_chemical_formula_weight         1529.98
_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
_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                90
_cell_angle_beta                 100.7350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.86970(10)
_cell_length_b                   28.1617(2)
_cell_length_c                   14.37940(10)
_cell_measurement_reflns_used    19588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.1480
_cell_measurement_theta_min      4.4300
_cell_volume                     3926.77(6)
_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(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -14.00   43.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 57

  2 omega    6.00   69.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -30.0000 63

  3 omega   29.00  123.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   37.0000  -30.0000 94

  4 omega   69.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 33

  5 omega   86.00  161.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000    0.0000 75

  6 omega   84.00  124.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  164.0000   71.0000 40

  7 omega   38.00  123.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 85

  8 omega   65.00   93.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -60.0000 28

  9 omega   53.00   89.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 36

 10 omega   51.00   96.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 45

 11 omega   90.00  116.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 26

 12 omega   55.00   81.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -180.0000 26

 13 omega   38.00   91.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -120.0000 53

 14 omega   38.00  142.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -90.0000 104

 15 omega   47.00  122.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 75

 16 omega   47.00   93.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 46

 17 omega   39.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   30.0000 51

 18 omega   36.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   90.0000 54

 19 omega   37.00   62.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  150.0000 25

 20 omega   36.00  174.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000  150.0000 138

 21 omega   36.00  112.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 76

 22 omega   26.00  110.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 84

 23 omega   35.00   69.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 34

 24 omega   35.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 55

 25 omega  -15.00   38.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 53

 26 omega  -10.00   66.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   90.0000 76

 27 omega  -76.00  -27.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  164.0000   71.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25894
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         67.487
_diffrn_reflns_theta_min         4.433
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72417
_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    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0655P)^2^+1.8992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6931
_reflns_number_total             7070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           tifrh012
_cod_database_code               4514940
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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:
 C9(H9), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.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), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C38(H38), C111(H111)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C222(H22A,H22B,H22C), C333(H33A,H33B,H33C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              36609
_shelx_hkl_checksum              57250
_olex2_submission_special_instructions 'No special instructions were received'