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_7223506
_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
'C90 H90 Br4 Dy2 N10 Ni2 O18, C84 H80 Br4 Dy2 N8 Ni2 O18, 4(Cl O4)'
_chemical_formula_sum            'C174 H170 Br8 Cl4 Dy4 N18 Ni4 O52'
_chemical_formula_weight         5011.19
_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                88.220(6)
_cell_angle_beta                 85.020(6)
_cell_angle_gamma                84.859(6)
_cell_formula_units_Z            1
_cell_length_a                   13.4199(5)
_cell_length_b                   19.4201(7)
_cell_length_c                   20.7033(15)
_cell_measurement_temperature    100
_cell_volume                     5352.1(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  2014ncs0568_info
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72585
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.059
_exptl_absorpt_coefficient_mu    3.340
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.601
_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)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.645
_refine_diff_density_min         -3.194
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         24304
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+5.6291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19517
_reflns_number_total             24304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           13_CCDC_1406229
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223506
_shelxl_version_number           2014-1
_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, All O(H,H) groups
2. Restrained distances
 N2-C12
 1.49 with sigma of 0.02
3. Others
 Fixed Sof: O17(0.5) O15(0.5)
4.a Rotating group:
 O0AA(H0AB,H0AC)
4.b Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C17(H17), C21(H21), C1(H1), C11(H11), C22(H22), C23(H23),
 C26(H26), C8(H8), C0AA(H0AA), C3(H3), C4(H4), C16(H16), C3AA(H3AA), C24(H24),
 C42(H42), C45(H45), C51(H51), C54(H54), C57(H57), C66(H66), C70(H70), C77(H77),
  C80(H80), C81(H81), C83(H83), C94(H94), C95(H95), C102(H102), C104(H104),
 C112(H112), C113(H113), C115(H115), C119(H119), C129(H129), C135(H135),
 C151(H151), C153(H153), C159(H159), C161(H161), C163(H163)
4.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C4AA(H4AA,H4AB,H4AC), C32(H32A,H32B,H32C), C27(H27A,H27B,
 H27C), C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C59(H59A,H59B,H59C),
 C107(H10A,H10B,H10C), C128(H12A,H12B,H12C), C146(H14A,H14B,H14C), C2(H2A,H2B,
 H2C), C12(H12D,H12E,H12F), C13(H13A,H13B,H13C), C1E(H1EA,H1EB,H1EC)
;
_shelx_res_checksum              27362
_olex2_submission_special_instructions 'No special instructions were received'