Controllable synthesis of two adenosine 5'-monophosphate nucleotide coordination polymers via pH regulation: crystal structure and chirality.
Song, Wen-Jing; Su, Hao; Zhou, Pei; Zhu, Yan-Hong; Khan, Maroof Ahmad; Song, Jian-Biao; Li, Hui; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4713–4719; doi:10.1039/d1dt00133g

data_7706753
_publ_section_title
;
 Controllable synthesis of two adenosine 5'-monophosphate nucleotide
 coordination polymers via pH regulation: crystal structure and chirality.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4713
_journal_page_last               4719
_journal_paper_doi               10.1039/d1dt00133g
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         '11(O), C40 H50 Cu2 N14 O18 P2, 2(N O3)'
_chemical_formula_sum            'C40 H50 Cu2 N16 O35 P2'
_chemical_formula_weight         1503.98
_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
_audit_creation_date             2020-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-06 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                65.39(3)
_cell_angle_beta                 68.66(3)
_cell_angle_gamma                80.04(3)
_cell_formula_units_Z            1
_cell_length_a                   10.493(2)
_cell_length_b                   12.782(3)
_cell_length_c                   13.595(3)
_cell_measurement_reflns_used    7096
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.27
_cell_measurement_theta_min      2.16
_cell_volume                     1543.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23071
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear  blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       Triclinic
_exptl_crystal_F_000             770
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ????'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 4320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.042(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         17225
_refine_ls_number_restraints     2415
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.695
_reflns_number_gt                14984
_reflns_number_total             17225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00133g2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7706753--7706754.cif.'
_cod_original_cell_volume        1543.7(7)
_cod_database_code               7706753
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6A of O6, {H15A,H15B} of O15, All C(H,H) groups, All N(H)
  groups, All N(H,H) groups
 At 1.5 times of:
  H6B of O6, H7B of O7, H9C of O9, H10A of O10, H19A of O19, H20A of O20,
  {H16A,H16B} of O16
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim
N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim N15 \\sim N16 \\sim O17 \\sim
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O18
\\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26
\\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34
\\sim O35: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
3.a Riding coordinates:
 O6(H6A,H6B), O15(H15A,H15B)
3.b Rotating group:
 O16(H16A,H16B)
3.c Ternary CH refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C32(H32), C33(H33), C34(H34), C35(H35)
3.d Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C31(H31A,H31B)
3.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C26(H26),
  C30(H30), C36(H36), C40(H40), N7(H7A), N13(H13A)
3.f X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N12(H12A,H12B)
3.g Idealised tetrahedral OH refined as rotating group:
 O7(H7B), O9(H9C), O10(H10A), O19(H19A), O20(H20A)
;
_shelx_res_checksum              24092
_shelx_hkl_checksum              93612
_olex2_submission_special_instructions 'No special instructions were received'