La(III) biodistribution profiles from intravenous and oral dosing of two lanthanum complexes, La(dpp)3 and La(XT), and evaluation as treatments for bone resorption disorders
Weekes, David M.; Cawthray, Jacqueline F.; Rieder, Meghanne; Syeda, Jaweria; Ali, Munawar; Wasan, Ellen; Kostelnik, Tom Kostelnik; Patrick, Brian O.; Panahifar, A.; Cooper, David M.L.; Al-Dissi, Ahmad; Wasan, Kishor; Orvig, Chris; Metallomics  (2017) –; doi:10.1039/C7MT00133A

data_1546104
_publ_section_title
;
 La(III) biodistribution profiles from intravenous and oral dosing of two
 lanthanum complexes, La(dpp)3 and La(XT), and evaluation as treatments
 for bone resorption disorders
;
_journal_name_full               Metallomics
_journal_paper_doi               10.1039/C7MT00133A
_journal_year                    2017
_chemical_formula_moiety         'C21 H28 La N3 O8, 11.75(H2 O)'
_chemical_formula_sum            'C21 H51.5 La N3 O19.75'
_chemical_formula_weight         801.06
_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
_audit_creation_date             2015-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                73.963(6)
_cell_angle_beta                 79.565(5)
_cell_angle_gamma                73.194(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8019(16)
_cell_length_b                   11.2323(15)
_cell_length_c                   15.296(2)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.65
_cell_volume                     1697.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22637
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.177
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0448 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.8991.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       prism
_exptl_crystal_F_000             827
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.036
_refine_diff_density_min         -4.168
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9777
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+3.7698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8869
_reflns_number_total             9777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7mt00133a1.cif
_cod_data_source_block           co488
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C21 H51.50 La N3 O19.75'
_cod_database_code               1546104
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.623
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O16) = Uanis(O16A)
Uanis(O17A) = Uanis(O17)
Uanis(O18) = Uanis(O18A)
Uanis(O15) = Uanis(O15A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O17)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(O17A)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(O18A)=Sof(H18C)=Sof(H18D)=1-FVAR(2)
 Sof(O18)=Sof(H18A)=Sof(H18B)=FVAR(2)
 Sof(O16A)=Sof(H16A)=Sof(H16B)=1-FVAR(3)
 Sof(O16)=Sof(H16C)=Sof(H16D)=FVAR(3)
 Sof(O8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(4)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
 Sof(O21)=Sof(H21D)=Sof(H21E)=1-FVAR(5)
 Sof(O19)=Sof(H19A)=Sof(H19B)=Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(5)
 Sof(O15A)=Sof(H15F)=Sof(H15G)=1-FVAR(6)
 Sof(O15)=Sof(H15D)=Sof(H15E)=FVAR(6)
 Fixed X: H15F(0.051) H15G(-0.06299)
 Fixed Y: H15F(1.03701) H15G(1.06702)
 Fixed Z: H15F(0.81283) H15G(0.87384)
5.a Free rotating group:
 O21(H21D,H21E), O18(H18A,H18B), O9(H9A,H9B), O17A(H17A,H17B), O10(H10A,H10B),
 O19(H19A,H19B), O11(H11A,H11B), O16A(H16A,H16B), O12(H12A,H12B), O17(H17C,
 H17D), O13(H13A,H13B), O18A(H18C,H18D), O14(H14D,H14E), O20(H20A,H20B),
 O15(H15D,H15E), O16(H16C,H16D)
5.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O8A(H8AA,H8AB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7C,H7D,H7E), C8(H8C,H8D,H8E), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              11279
_shelx_hkl_checksum              55336
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'