Studies on the structure and chirality of A-motif in adenosine monophosphate nucleotide metal coordination complexes
Iqbal, Muhammad Javed; Li, Zhongkui; Khan, Maroof Ahmad; Zhu, Yanhong; Hussain, Wajid; Su, Hao; Qiu, Qi-Ming; Shoukat, Rizwan; Li, Hui; CrystEngComm 23 (2021) 4175–4180; doi:10.1039/D1CE00276G

data_7242803
_publ_section_title
;
 Studies on the structure and chirality of A-motif in adenosine
 monophosphate nucleotide metal coordination complexes
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4175
_journal_page_last               4180
_journal_paper_doi               10.1039/D1CE00276G
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H28 Cd N7 O10 P, 2(H2 O), 5(O)'
_chemical_formula_sum            'C22 H42 Cd N7 O17 P'
_chemical_formula_weight         819.99
_chemical_name_systematic        amp-cd-bpe
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                111.040(2)
_cell_angle_beta                 93.282(2)
_cell_angle_gamma                92.104(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8541(5)
_cell_length_b                   10.2632(7)
_cell_length_c                   14.0271(10)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.98
_cell_volume                     917.70(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12548
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.622
_diffrn_reflns_theta_min         2.130
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       plate
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 4614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         10115
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.434
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.753
_reflns_number_gt                10096
_reflns_number_total             10115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00276g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7242802--7242804.cif.'
_cod_database_code               7242803
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H7B-N7
 2.12 with sigma of 0.02
 H14-C14
 2.12 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Free rotating group:
 O11(H11A,H11B), O13(H13C,H13D)
4.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B)
4.c Ternary CH refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C23(H23)
4.d Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
4.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9A), C10(H10), C11(H11),
 C12(H12), C17(H17), C20(H20)
4.f X=CH2 refined with riding coordinates:
 N7(H7A,H7B)
4.g Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 45 electrons were
found in a volume of 91\%A^3 in 1 void per unit cell.
This is consistent with the presence of 
4.5[H2O] per Formula Unit 
which account for 45 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95547
_shelx_hkl_checksum              96217
_shelx_fab_checksum              78635
_olex2_submission_special_instructions 'No special instructions were received'