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_4514933
_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         'C36 H34 O4 P, C3 H7 N O, C3 H5 N2'
_chemical_formula_sum            'C42 H46 N3 O5 P'
_chemical_formula_weight         703.79
_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                88.912(2)
_cell_angle_beta                 88.455(2)
_cell_angle_gamma                89.894(2)
_cell_formula_units_Z            4
_cell_length_a                   9.4329(6)
_cell_length_b                   15.1034(10)
_cell_length_c                   26.0725(18)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.55
_cell_volume                     3712.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            49517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1601 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.7854. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.085
_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     930
_refine_ls_number_reflns         15345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0481P)^2^+16.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11039
_reflns_number_total             15345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03192_si_002.cif
_cod_data_source_block           18jund_0m
_cod_database_code               4514933
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9285(14)
 0.0715(14)
2. 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
3.a Ternary CH refined with riding coordinates:
 C21(H21), C36(H36), C54(H54), C85(H85)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C4(H4), C5(H5), C12(H12), C10(H10), C9(H9), C3(H3), C8(H8),
 C11(H11), C19(H19), C18(H18), C16(H16), C15(H15), C17(H17), C26(H26), C24(H24),
  C29(H29), C31(H31), C35(H35), C34(H34), C32(H32), C33(H33), C78(H78),
 C77(H77), C79(H79), N5(H5A), N6(H6B), C42(H42), C44(H44), C43(H43), C38(H38),
 C39(H39), C41(H41), C40(H40), C46(H46), C47(H47), C53(H53), C49(H49), C52(H52),
  C50(H50), C51(H51), C55(H55), C60(H60), C63(H63), C59(H59), C62(H62),
 C61(H61), C69(H69), C70(H70), C83(H83), C66(H66), C65(H65), C64(H64), N3(H3A),
 N2(H2A)
3.c Tetrahedral OH refined with riding coordinates:
 O6(H6A), O10(H10A)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C80(H80A,H80B,H80C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C74(H74A,
 H74B,H74C), C76(H76A,H76B,H76C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              66964
_shelx_hkl_checksum              33221
_olex2_submission_special_instructions 'No special instructions were received'