Bis(4-carboxylpyrazol-1-yl)acetic acid: a scorpionate ligand for complexes with improved water solubility.
Tzegai, Wintana; Reil, Michaela; Burzlaff, Nicolai; Dalton transactions (Cambridge, England : 2003) 51 (2022) 6839–6845; doi:10.1039/d2dt00848c

data_7710172
_publ_section_title
;
 Bis(4-carboxylpyrazol-1-yl)acetic acid: a scorpionate ligand for
 complexes with improved water solubility.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6839
_journal_page_last               6845
_journal_paper_doi               10.1039/d2dt00848c
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C13 H7 N4 O9 Re, 0.5(H2 O)'
_chemical_formula_sum            'C13 H8 N4 O9.5 Re'
_chemical_formula_weight         558.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                107.251(3)
_cell_angle_beta                 94.748(3)
_cell_angle_gamma                110.515(3)
_cell_formula_units_Z            8
_cell_length_a                   14.3811(5)
_cell_length_b                   15.1010(5)
_cell_length_c                   17.2257(6)
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.2770
_cell_measurement_theta_min      3.3090
_cell_volume                     3272.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -109.00 -17.00   1.00    5.00    --  -40.61 -38.00   0.00   92
  2  \w   -115.00 -19.00   1.00    5.00    --  -40.61 -38.00 -90.00   96
  3  \w      6.00  78.00   1.00    5.00    --   40.61 -99.00  60.00   72
  4  \w    -21.00  73.00   1.00    5.00    --   40.61 -77.00-180.00   94
  5  \w     30.00 128.00   1.00   20.00    --  104.57 -30.00-150.00   98
  6  \w     28.00  55.00   1.00   20.00    --  104.57-111.00  90.00   27
  7  \w     80.00 173.00   1.00   20.00    --  104.57  45.00-120.00   93
  8  \w     29.00 117.00   1.00   20.00    --  104.57 -77.00-180.00   88
  9  \w     71.00 109.00   1.00   20.00    --  104.57-111.00  90.00   38
 10  \w     23.00 106.00   1.00   20.00    --  104.57 -94.00 150.00   83
 11  \w     32.00 134.00   1.00   20.00    --  104.57 -61.00 -30.00  102
 12  \w    123.00 159.00   1.00   20.00    --  104.57  77.00-180.00   36
 13  \w     56.00 109.00   1.00   20.00    --  104.57-111.00 -30.00   53
 14  \w     27.00 130.00   1.00   20.00    --  104.57 -15.00  60.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1156875000
_diffrn_orient_matrix_UB_12      -0.0298128000
_diffrn_orient_matrix_UB_13      -0.0178049000
_diffrn_orient_matrix_UB_21      0.0142515000
_diffrn_orient_matrix_UB_22      0.1015528000
_diffrn_orient_matrix_UB_23      0.0651170000
_diffrn_orient_matrix_UB_31      0.0095729000
_diffrn_orient_matrix_UB_32      0.0480264000
_diffrn_orient_matrix_UB_33      -0.0679117000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21454
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.529
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.146
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         12476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.6826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10901
_reflns_number_total             12476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00848c2.cif
_cod_data_source_block           buni211203a
_cod_original_formula_sum        'C13 H8 N4 O9.50 Re'
_cod_database_code               7710172
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H8N4O9.5Re
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C101(H101), C301(H301), C1(H1), C201(H201)
2.c Aromatic/amide H refined with riding coordinates:
 C324(H324), C224(H224), C114(H114), C222(H222), C314(H314), C14(H14),
 C212(H212), C12(H12), C322(H322), C122(H122), C24(H24), C214(H214), C112(H112),
  C22(H22), C124(H124), C312(H312)
2.d Idealised tetrahedral OH refined as rotating group:
 O321(H321), O111(H111), O11(H11), O121(H121), O311(H311), O221(H221), O21(H21)
;
_shelx_res_checksum              23404
_olex2_date_sample_data_collection 2021-12-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.456
_oxdiff_exptl_absorpt_empirical_full_min 0.632