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_7232885
_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_formula_moiety         'C16 H30 Cu N4 O16 P4'
_chemical_formula_sum            'C16 H30 Cu N4 O16 P4'
_chemical_formula_weight         721.86
_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   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                95.54(3)
_cell_angle_beta                 93.89(3)
_cell_angle_gamma                92.28(3)
_cell_formula_units_Z            1
_cell_length_a                   6.862(4)
_cell_length_b                   9.864(5)
_cell_length_c                   9.939(5)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      2.848
_cell_volume                     667.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20945
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            greenish
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plate
_exptl_crystal_F_000             371
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3418
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0501P)^2^+0.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2916
_reflns_number_total             3418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00614a2.cif
_cod_data_source_block           tr26015a
_cod_depositor_comments
'Adding full bibliography for 7232883--7232885.cif.'
_cod_database_code               7232885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              62152