Self-assembly of bis-β-diketone-based [M2L2] dinuclear platforms into 2-dimensional coordination polymers
Brock, A. J.; McMurtrie, John C.; Clegg, J. K.; CrystEngComm 21 (2019) 4786–; doi:10.1039/C9CE00896A

data_7233133
_publ_section_title
;
 Self-assembly of bis-\b-diketone-based [M2L2] dinuclear platforms into
 2-dimensional coordination polymers
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4786
_journal_paper_doi               10.1039/C9CE00896A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C19 H25 N O4'
_chemical_formula_sum            'C19 H25 N O4'
_chemical_formula_weight         331.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-05-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-07 deposited with the CCDC.    2019-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.993(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2281(5)
_cell_length_b                   19.4672(19)
_cell_length_c                   15.2664(13)
_cell_measurement_reflns_used    1705
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      64.8320
_cell_measurement_theta_min      4.5340
_cell_volume                     1840.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0696
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  90.00   1.00    6.25    --   34.64  57.00   0.00   70
  2  \w     49.00 102.00   1.00    6.25    --   34.64  77.00 -90.00   53
  3  \w     83.00 156.00   1.00    9.00    --   98.65  50.00   0.00   73
  4  \w     98.00 124.00   1.00    9.00    --   98.65 -50.00 -90.00   26
  5  \w     60.00 100.00   1.00    9.00    --   98.65 -77.00-150.00   40
  6  \w     33.00  85.00   1.00    9.00    --   98.65-112.00-150.00   52
  7  \w     28.00  86.00   1.00    9.00    --   98.65 -50.00 -90.00   58
  8  \w     29.00  55.00   1.00    9.00    --   98.65-100.00-134.00   26
  9  \w    -18.00  72.00   1.00    6.25    --   34.64 -99.00-120.00   90
 10  \w     32.00  92.00   1.00    6.25    --   34.64  57.00 150.00   60
 11  \w     79.00 168.00   1.00    9.00    --   98.65 112.00-150.00   89
 12  \w     92.00 152.00   1.00    9.00    --   98.65 112.00-180.00   60
 13  \w     43.00  68.00   1.00    9.00    --   98.65 178.00  60.00   25
 14  \w    106.00 133.00   1.00    9.00    --   98.65 178.00  60.00   27
 15  \w     26.00  52.00   1.00    9.00    --   98.65-112.00 150.00   26
 16  \w     54.00  90.00   1.00    9.00    --   98.65-112.00 150.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5919
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        65.156
_diffrn_reflns_theta_max         65.156
_diffrn_reflns_theta_min         3.692
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.196
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3073
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0906P)^2^+0.1255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2260
_reflns_number_total             3073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00896a2.cif
_cod_data_source_block           jkc16ab03
_cod_depositor_comments
'Adding full bibliography for 7233133--7233136.cif.'
_cod_database_code               7233133
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O002-H002
 0.83 with sigma of 0.02
 O001-H001
 0.83 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C00O, C00N, C3AA, C00M, C2A, C2, C00I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AA, C00L, C00J, C2AA, C00K, C0AA, C00H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(C00J)=Sof(H00A)=Sof(H00F)=Sof(H00G)=Sof(C00K)=Sof(H00H)=Sof(H00I)=
 Sof(H00J)=Sof(C00L)=Sof(H00K)=Sof(H00L)=Sof(H00M)=FVAR(1)
 Sof(C2A)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=Sof(C00O)=Sof(H00T)=Sof(H00U)=
 Sof(H00V)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(2)
 Sof(C00M)=Sof(H00N)=Sof(H00O)=Sof(H00P)=Sof(C00N)=Sof(H00Q)=Sof(H00R)=
 Sof(H00S)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E)
5.b Idealised Me refined as rotating group:
 C00J(H00A,H00F,H00G), C00K(H00H,H00I,H00J), C00L(H00K,H00L,H00M), C00M(H00N,
 H00O,H00P), C00N(H00Q,H00R,H00S), C2(H2A,H2B,H2C), C0AA(H0AA,H0AB,H0AC),
 C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C2A(H2AD,H2AE,H2AF), C00O(H00T,
 H00U,H00V), C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              89288
_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
;