Deciphering preferred solid-state conformations in nitrogen-containing bisphosphonates and their coordination compounds. A case study of discrete Cu(ii) complexes based on Cα-substituted analogues of zoledronic acid: crystal structures and solid-state characterization
Rojek, Tomasz; Goldeman, Waldemar; Ślepokura, Katarzyna; Zierkiewicz, Wiktor; Matczak-Jon, Ewa; CrystEngComm 21 (2019) 4340–; doi:10.1039/C9CE00614A

data_7232883
_publ_section_title
;
 Deciphering preferred solid-state conformations in nitrogen-containing
 bisphosphonates and their coordination compounds. A case study of
 discrete Cu(ii) complexes based on C\a-substituted analogues of
 zoledronic acid: crystal structures and solid-state characterization
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4340
_journal_paper_doi               10.1039/C9CE00614A
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H28 Cu N4 O15 P4, 8(H2 O)'
_chemical_formula_sum            'C14 H44 Cu N4 O23 P4'
_chemical_formula_weight         823.95
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-18 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                92.09(3)
_cell_angle_beta                 90.88(3)
_cell_angle_gamma                114.23(3)
_cell_formula_units_Z            1
_cell_length_a                   7.958(3)
_cell_length_b                   9.582(3)
_cell_length_c                   11.270(4)
_cell_measurement_reflns_used    4907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.68
_cell_measurement_theta_min      2.88
_cell_volume                     782.7(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.535
_diffrn_measurement_device_type  'Kuma KM4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.535
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.765
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       plate
_exptl_crystal_F_000             429
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.725
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.197(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0833P)^2^+0.1082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.535
_reflns_number_gt                5527
_reflns_number_total             5747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00614a2.cif
_cod_data_source_block           tr08113
_cod_depositor_comments
'Adding full bibliography for 7232883--7232885.cif.'
_cod_original_formula_sum        ' C14 H44 Cu N4 O23 P4'
_cod_database_code               7232883
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              74673