Crystal structure of poly-[triaqua-(μ4-5′-carboxy-[1,1′-biphenyl]-2,3,3′-tricarboxylate-κ6 O 1,O 2:O 3,O 4:O 5:O 6)praseodymium(III), C16H13O11Pr
Li, Rong Fang; Liu, Xin Fang; Feng, Xun; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 3–5; doi:10.1515/ncrs-2016-0071

data_8106411
_publ_section_title
;
 Crystal structure of
 poly-[triaqua-(\m4-5&#x2032;-carboxy-[1,1&#x2032;-biphenyl]-2,3,3&#x2032;-tricarboxylate-\k6
 O 1,O 2:O 3,O 4:O 5:O 6)praseodymium(III), C16H13O11Pr
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              3
_journal_page_last               5
_journal_paper_doi               10.1515/ncrs-2016-0071
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C16 H13 O11 Pr'
_chemical_formula_sum            'C16 H13 O11 Pr'
_chemical_formula_weight         522.17
_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
_cell_angle_alpha                94.137(2)
_cell_angle_beta                 101.152(2)
_cell_angle_gamma                96.831(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9159(4)
_cell_length_b                   10.8953(6)
_cell_length_c                   11.6439(7)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      3.030
_cell_volume                     850.61(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16557
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         3.030
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.8907.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            olivine
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0212P)^2^+2.9812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3448
_reflns_number_total             3889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0071_suppl.cif
_cod_data_source_block           ww
_cod_database_code               8106411
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H9A of O9
 At 1.5 times of:
  All O(H,H) groups, H9B of O9, H6 of O6
2.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C12(H12), C14(H14)
2.c Tetrahedral OH refined with riding coordinates:
 O6(H6)
;
_shelx_res_checksum              19486
_shelx_hkl_checksum              68986
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'