Crystal structure of [(bis(1,10-phenanthroline-κ2 N,N′)-(2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-κ2O:O′))nickel(II) monohydrate, (1,10-phenanthroline-κ2 N:N′)-(μ2-(5-(3′,4′-dicarboxylphenoxy)-isophthalate-κ2O:O′))nickel(II)], C40H24N4O9Ni ⋅ H2O
Yao, Li-Ping; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1133–1134; doi:10.1515/ncrs-2020-0201

data_8105399
_publ_section_title
;
 Crystal structure of [(bis(1,10-phenanthroline-\k2
 N,N&#x2032;)-(2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-\k2O:O&#x2032;))nickel(II)
 monohydrate, (1,10-phenanthroline-\k2
 N:N&#x2032;)-(\m2-(5-(3&#x2032;,4&#x2032;-dicarboxylphenoxy)-isophthalate-\k2O:O&#x2032;))nickel(II)],
 C40H24N4O9Ni &#x22C5; H2O
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1133
_journal_page_last               1134
_journal_paper_doi               10.1515/ncrs-2020-0201
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C40 H24 N4 Ni O9'
_chemical_formula_sum            'C40 H24 N4 Ni O9'
_chemical_formula_weight         763.34
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.440(5)
_cell_angle_beta                 77.913(6)
_cell_angle_gamma                76.014(6)
_cell_formula_units_Z            2
_cell_length_a                   11.5851(8)
_cell_length_b                   11.5875(7)
_cell_length_c                   13.3921(8)
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    289.07(10)
_cell_measurement_theta_max      25.3790
_cell_measurement_theta_min      3.7020
_cell_volume                     1696.65(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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_environment      air
_diffrn_ambient_temperature      289.07(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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    -20.00  29.00   1.00    2.00    --   -9.62 -99.00 -60.00   49
  2  \w    -20.00  50.00   1.00    2.00    --   10.64 -99.00 -90.00   70
  3  \w     -6.00  78.00   1.00    2.00    --   10.64  57.00   0.00   84
  4  \w    -57.00  37.00   1.00    2.00    --   10.64 -77.00-180.00   94
  5  \w     -6.00  78.00   1.00    2.00    --   10.64  57.00  90.00   84
  6  \w    -29.00  54.00   1.00    2.00    --   -9.62  38.00  30.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286932000
_diffrn_orient_matrix_UB_12      -0.0179247000
_diffrn_orient_matrix_UB_13      -0.0491833000
_diffrn_orient_matrix_UB_21      0.0004214000
_diffrn_orient_matrix_UB_22      0.0604432000
_diffrn_orient_matrix_UB_23      -0.0189272000
_diffrn_orient_matrix_UB_31      0.0573756000
_diffrn_orient_matrix_UB_32      -0.0069189000
_diffrn_orient_matrix_UB_33      0.0137279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15923
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         5769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.5998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                4660
_reflns_number_total             5769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0201_suppl.cif
_cod_data_source_block           181
_cod_original_cell_volume        1696.65(18)
_cod_database_code               8105399
_chemical_oxdiff_formula         'c h n o ni'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C6(H6), C7(H7A), C9(H9), C11(H11), C13(H13), C17(H17), C18(H18),
 C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40)
2.b Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7)
;
_olex2_date_sample_data_collection 2017-10-14
_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 1.439
_oxdiff_exptl_absorpt_empirical_full_min 0.678