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_7710174
_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         'C12 H7 Cl N4 O8 Ru, H2 O'
_chemical_formula_sum            'C12 H9 Cl N4 O9 Ru'
_chemical_formula_weight         489.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-11
_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                90
_cell_angle_beta                 93.0360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5010(2)
_cell_length_b                   14.0811(2)
_cell_length_c                   9.18410(10)
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.4800
_cell_measurement_theta_min      5.7430
_cell_volume                     1614.39(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.963
_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   -112.00 -40.00   1.00    1.00    --  -41.69 -38.00 -90.00   72
  2  \w    -21.00  74.00   1.00    1.00    --   41.69 -77.00 150.00   95
  3  \w     23.00 102.00   1.00    4.00    --  104.37 -94.00 -60.00   79
  4  \w    108.00 150.00   1.00    4.00    --  104.37 125.00-150.00   42
  5  \w     61.00 106.00   1.00    4.00    --  104.37 -94.00  30.00   45
  6  \w     56.00 174.00   1.00    4.00    --  104.37  15.00 -30.00  118
  7  \w     87.00 112.00   1.00    4.00    --  104.37-125.00 -90.00   25
  8  \w     35.00  60.00   1.00    4.00    --  104.37-125.00 -90.00   25
  9  \w     32.00 127.00   1.00    4.00    --  104.37 -45.00 -60.00   95
;
_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      0.0011899000
_diffrn_orient_matrix_UB_12      0.1090717000
_diffrn_orient_matrix_UB_13      -0.0138049000
_diffrn_orient_matrix_UB_21      0.0046594000
_diffrn_orient_matrix_UB_22      -0.0090316000
_diffrn_orient_matrix_UB_23      -0.1667137000
_diffrn_orient_matrix_UB_31      -0.1232677000
_diffrn_orient_matrix_UB_32      0.0007414000
_diffrn_orient_matrix_UB_33      -0.0151481000
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5952
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.586
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.973
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0458P)^2^+1.4266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2970
_reflns_number_total             3100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00848c2.cif
_cod_data_source_block           buni211221a
_cod_database_code               7710174
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H7ClN4O9Ru
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O11-H11 = O21-H21
 0.8 with sigma of 0.02
 O21-H21 \\sim O11-H11
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O4 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C3 \\sim O3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
C4 \\sim O4: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
4. Rigid body (RIGU) restrains
 H13a, O13, H13b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C24(H24), C14(H14)
;
_shelx_res_checksum              21429
_olex2_date_sample_data_collection 2021-12-21
_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 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.756