Structural diversity in cobalt camphorate coordination polymers with flexible dipyridylamide ligands including looped layers and self-penetrated topologies
Przybyla, Jack J.; Ezenyilimba, Frederick C.; LaDuca, Robert L.; Inorganica Chimica Acta 498 (2019) 119087–; doi:10.1016/j.ica.2019.119087

data_1565732
_publ_section_title
;
 Structural diversity in cobalt camphorate coordination polymers with
 flexible dipyridylamide ligands including looped layers and
 self-penetrated topologies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119087
_journal_paper_doi               10.1016/j.ica.2019.119087
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C36 H46 Co2 N4 O10, 2(H2 O)'
_chemical_formula_sum            'C36 H50 Co2 N4 O12'
_chemical_formula_weight         848.66
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.146(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.681(7)
_cell_length_b                   12.340(4)
_cell_length_c                   13.694(4)
_cell_measurement_reflns_used    8981
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.40
_cell_volume                     3833(2)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30253
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.361
_diffrn_reflns_theta_min         1.796
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0610 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.9020. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0812
_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^)+23.0643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5077
_reflns_number_total             7014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_database_code               1565732
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,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(C25) = Uanis(C21) = Uanis(N3) = Uanis(C24) = Uanis(C20) = Uanis(C19) =
Uanis(C23) = Uanis(C22) = Uanis(C18) = Uanis(N2)
3. Others
 Fixed Sof: H2B(0.5) H2A(0.5) H3B(0.5) H3A(0.5) H2(0.5) H5(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5) H33(0.5)
 H36(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5)
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C33(H33), C36(H36)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3C,H3D), C4(H4A,H4B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C34(H34A,H34B), C35(H35A,H35B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2B), N2(H2A), N3(H3B), N3(H3A), C12(H12), C13(H13), C15(H15), C16(H16),
 C27(H27), C28(H28), C30(H30), C31(H31)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'