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_7242804
_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
'C32 H40 Cd N12 O14 P2, C12 H10 N2, C O, 4(O)'
_chemical_formula_sum            'C45 H62 Cd N14 O19 P2'
_chemical_formula_weight         1277.42
_chemical_name_systematic        damp-cd-bpe-MI-343
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9986(5)
_cell_length_b                   19.9756(7)
_cell_length_c                   10.1006(4)
_cell_measurement_reflns_used    8587
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.26
_cell_volume                     2824.44(18)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_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    'SHELXS  (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.942
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.514
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6997
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1513 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.9377.
The \l/2 correction factor is 0.0015.
;
_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    1.502
_exptl_crystal_description       cube
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 2604 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                6976
_reflns_number_total             8618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00276g2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7242802--7242804.cif.'
_cod_database_code               7242804
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.875
_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. Uiso/Uaniso restraints and constraints
Uanis(C12A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: C12B(0.75) H12B(0.75) C12A(0.25) H12A(0.25) O8(0.5) C23(0.5)
 O9(0.5) O11(0.5)
4.a Rotating group:
 O1(H1A,H1B)
4.b Ternary CH refined with riding coordinates:
 C14(H14), C15(H15), C17(H17)
4.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C18(H18), C21(H21), C7(H7C), C8(H8),
 C11(H11), C12B(H12B), C12A(H12A)
4.e Tetrahedral OH refined with riding coordinates:
 O3(H3)
4.f X=CH2 refined with riding coordinates:
 N7(H7A,H7B)
4.g Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              28594
_shelx_hkl_checksum              7391
_olex2_submission_special_instructions 'No special instructions were received'