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_7230987
_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         'C27 H12 Cu N3 O12, C3 H7 N O, C2 H8 N'
_chemical_formula_sum            'C32 H27 Cu N5 O13'
_chemical_formula_weight         753.12
_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
_audit_creation_date             2018-01-25
_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                113.74(3)
_cell_angle_beta                 98.29(3)
_cell_angle_gamma                92.58(3)
_cell_formula_units_Z            2
_cell_length_a                   9.864(2)
_cell_length_b                   13.216(3)
_cell_length_c                   13.312(3)
_cell_measurement_reflns_used    57978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.652
_cell_measurement_theta_min      1.694
_cell_volume                     1561.7(7)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 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 0.986
_diffrn_measured_fraction_theta_max 0.832
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57978
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.656
_diffrn_reflns_theta_min         1.694
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_recrystallization_method
'Crystallised at elevated temperature from synthesis'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8771
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+1.7457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7041
_reflns_number_total             8771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00744f2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7230978--7230987.cif.'
_cod_original_cell_volume        1561.7(6)
_cod_database_code               7230987
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.985
_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, All N(H,H) groups
2. Restrained distances
 N4-C30
 1.45 with sigma of 0.01
 O13-C28
 1.25 with sigma of 0.005
 N5-H5A = N5-H5B
 0.91 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C12(H12), C25(H25), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              43915
_olex2_submission_special_instructions 'No special instructions were received'