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_7230986
_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         'C36 H16 N4 O16 Zn, 2(C2 H8 N)'
_chemical_formula_sum            'C40 H32 N6 O16 Zn'
_chemical_formula_weight         918.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 102.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.468(3)
_cell_length_b                   9.1690(18)
_cell_length_c                   25.512(5)
_cell_measurement_reflns_used    31341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      .632
_cell_volume                     3767.4(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1468
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_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         2.769
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1543P)^2^+6.4826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2826
_reflns_number_total             4324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00744f2.cif
_cod_data_source_block           2zn
_cod_depositor_comments
'Adding full bibliography for 7230978--7230987.cif.'
_cod_original_cell_volume        3767.4(14)
_cod_database_code               7230986
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.993
_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, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), N3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              37979
_olex2_submission_special_instructions 'No special instructions were received'