Isoskeletal Schiff base polynuclear coordination clusters: synthetic and theoretical aspects
Griffiths, Kieran; Dokorou, Vassiliki N.; Spencer, John; Abdul-Sada, Alaa; Vargas, Alfredo; Kostakis, George E.; CrystEngComm 18 (2016) 704–; doi:10.1039/C5CE02109J

data_7223512
_publ_section_title
;
 Isoskeletal Schiff base polynuclear coordination clusters: synthetic and
 theoretical aspects
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              704
_journal_paper_doi               10.1039/C5CE02109J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C88 H76 Co2 Dy2 N12 O30, 2(C3 H7 N O)'
_chemical_formula_sum            'C94 H90 Co2 Dy2 N14 O32'
_chemical_formula_weight         2370.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                106.940(3)
_cell_angle_beta                 91.065(2)
_cell_angle_gamma                97.754(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7821(9)
_cell_length_b                   13.5743(10)
_cell_length_c                   14.1583(10)
_cell_measurement_temperature    100
_cell_volume                     2324.2(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37052
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         2.490
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.803
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10595
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+3.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9688
_reflns_number_total             10595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           19_CCDC_1406235
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223512
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O1, N2, C3, C6, C7
 with sigma of 0.1
3. Rigid bond restraints
 C6, O1, C7, N2, H7, C3, H3A, H3B, H3C, H6A, H6B, H6C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C7 \\sim N2 \\sim H7 \\sim C3 \\sim H3A \\sim H3B \\sim H3C \\sim H6A
\\sim H6B \\sim H6C \\sim C6: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O1, C7, N2, H7, C3, H3A, H3B, H3C, H6A, H6B, H6C, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C32(0.5) H32(0.5) C9(0.5) H9A(0.5) H9B(0.5) C32A(0.5) H32A(0.5)
 C9A(0.5) H9AA(0.5) H9AB(0.5) H2AA(0.5) H2AB(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
7.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C45(H45A,H45B,H45C), C68(H68A,H68B,
 H68C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
7.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C0AA(H0AA), C16(H16), C8(H8), C15(H15), C18(H18), C1(H1), C25(H25),
 C32(H32), C2(H2), C4(H4), C40(H40), C41(H41), C54(H54), C62(H62), C69(H69),
 C73(H73), C75(H75), C77(H77), C32A(H32A), C7(H7)
7.d X=CH2 refined with riding coordinates:
 C79(H79A,H79B), C9(H9A,H9B), C9A(H9AA,H9AB)
;
_shelx_res_checksum              66436
_olex2_submission_special_instructions 'No special instructions were received'