New coordination networks containing trinuclear lanthanide complexes and hexacyanometallates.
Escobedo-Cruz, Francisco V; Hughbanks, Timothy; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6831–6841; doi:10.1039/c7dt02541f

data_7702142
_publ_section_title
;
 New coordination networks containing trinuclear lanthanide complexes and
 hexacyanometallates.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6831
_journal_page_last               6841
_journal_paper_doi               10.1039/c7dt02541f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H56 Co Er3 N12 O10'
_chemical_formula_sum            'C30 H56 Co Er3 N12 O10'
_chemical_formula_weight         1305.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.591(9)
_cell_length_b                   12.863(5)
_cell_length_c                   16.091(6)
_cell_measurement_reflns_used    6561
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.29
_cell_volume                     5090(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48261
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.841
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.269
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1334 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.7302.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       needle
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.7834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3652
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02541f1.cif
_cod_data_source_block           C30H56N12O10Er3Co
_cod_database_code               7702142
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.195
_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. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C1BA)
Uanis(C8) = Uanis(C2AA)
Uanis(C4) = Uanis(N2)
3.a Rotating group:
 O4(H4a,H4b), O1AA(H1Aa,H1Ab)
3.b Ternary CH refined with riding coordinates:
 C0AA(H0AA), C3AA(H3AA), C2AA(H2AA), C8(H8), C4AA(H4AA), C6(H6), C0BA(H0BA),
 C1BA(H1BA)
3.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6AA(H6Aa,H6Ab,H6Ac), C7AA(H7Aa,H7Ab,H7Ac), C8AA(H8Aa,H8Ab,
 H8Ac), C10(H10a,H10b,H10c), C1(H1a,H1b,H1c)
;
_shelx_res_checksum              6916
_shelx_fab_checksum              14601
_olex2_submission_special_instructions 'No special instructions were received'