Crystal structure of poly[(m3-3-carboxyadamantane-1-carboxylato-κ3 O:O′:O″)-(phenanthroline-κ2 N,N′)sodium(II)], C24H23N2NaO4
Li-Hua, Wang; Li-Li, Liu; Shu-Hua, Cao; Xi-Shi, Tai; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 745–747; doi:10.1515/ncrs-2021-0067

data_8104699
_publ_section_title
;
 Crystal structure of poly[(m3-3-carboxyadamantane-1-carboxylato-\k3
 O:O&#x2032;:O&#x2033;)-(phenanthroline-\k2 N,N&#x2032;)sodium(II)],
 C24H23N2NaO4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              745
_journal_page_last               747
_journal_paper_doi               10.1515/ncrs-2021-0067
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H23 N2 Na O4'
_chemical_formula_sum            'C24 H23 N2 Na O4'
_chemical_formula_weight         426.43
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.881(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5246(5)
_cell_length_b                   22.554(2)
_cell_length_c                   11.3358(9)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.3180
_cell_measurement_theta_min      2.5340
_cell_volume                     1922.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -83.00  21.00   1.00    5.50    --  -11.59 -77.00-150.00  104
  2  \w     56.00  81.00   1.00    5.50    --   11.74  37.00 -90.00   25
  3  \w     35.00  98.00   1.00    5.50    --   11.74-178.00  90.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0003271000
_diffrn_orient_matrix_UB_12      -0.0165045000
_diffrn_orient_matrix_UB_13      0.0532686000
_diffrn_orient_matrix_UB_21      0.0909974000
_diffrn_orient_matrix_UB_22      0.0071018000
_diffrn_orient_matrix_UB_23      0.0103883000
_diffrn_orient_matrix_UB_31      -0.0247167000
_diffrn_orient_matrix_UB_32      0.0258362000
_diffrn_orient_matrix_UB_33      0.0311496000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8172
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.012
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0458P)^2^+0.3454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2495
_reflns_number_total             3372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0067_suppl.cif
_cod_data_source_block           w5
_cod_database_code               8104699
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.986
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B), C17(H17A,H17B), C23(H23A,
 H23B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C10(H10), C11(H11), C9(H9), C8(H8), C3(H3), C12(H12)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;