Structural changes in coordination polymers in response to small changes in steric bulk (H vs. Me): an experimental and theoretical study
Kyratzis, Nicholas; Cao, Winnie; Izgorodina, Ekaterina I.; Turner, David R.; CrystEngComm 20 (2018) 4115–; doi:10.1039/C8CE00744F

data_7230978
_publ_section_title
;
 Structural changes in coordination polymers in response to small changes
 in steric bulk (H vs. Me): an experimental and theoretical study
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4115
_journal_paper_doi               10.1039/C8CE00744F
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C90 H77 Co4 N14 O39.5'
_chemical_formula_sum            'C90 H77 Co4 N14 O39.5'
_chemical_formula_weight         2222.37
_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   geom
_audit_creation_date             2018-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-30 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.09(3)
_cell_angle_beta                 100.49(3)
_cell_angle_gamma                115.21(3)
_cell_formula_units_Z            2
_cell_length_a                   15.060(3)
_cell_length_b                   17.240(3)
_cell_length_c                   18.790(4)
_cell_measurement_reflns_used    128774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      1.111
_cell_volume                     4304(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluICE (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            128774
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.111
_diffrn_source                   'MX1 Beamline Asutralian Synchrotron'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             2278
_exptl_crystal_recrystallization_method
'Crystallised at elevated temperature from synthesis'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.839
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1387
_refine_ls_number_reflns         19677
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0880
_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^)+(0.1807P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2352
_refine_ls_wR_factor_ref         0.2699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12145
_reflns_number_total             19677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00744f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7230978--7230987.cif.'
_cod_original_cell_volume        4304.1(18)
_cod_original_formula_sum        'C90 H77 Co4 N14 O39.50'
_cod_database_code               7230978
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C79-O35
 1.3 with sigma of 0.02
 C84-N10
 1.45 with sigma of 0.02
 N10-O35
 2.27 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N10, C79, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N9)=Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=Sof(H82C)=1-FVAR(1)
 Sof(N10)=Sof(C79)=Sof(H79)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=Sof(H84C)=FVAR(1)
 Fixed Sof: O34(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C20(H20A,H20B), C35(H35A,H35B), C38(H38A,H38B),
 C53(H53A,H53B), C56(H56A,H56B), C71(H71A,H71B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12), C25(H25), C27(H27), C28(H28), C30(H30),
 C43(H43), C45(H45), C46(H46), C48(H48), C61(H61), C63(H63), C64(H64), C66(H66),
  C74(H74), C79(H79), C80(H80), C85(H85), C88(H88), C91(H91), C94(H94)
5.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C),
 C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              4612
_olex2_submission_special_instructions 'No special instructions were received'