Coordination polymers from a flexible alkyldiamine-derived ligand
Emerson, Adrian; Hawes, Chris Samuel; Knowles, Gregory P.; Chaffee, Alan L.; Batten, Stuart R.; Turner, David Roger; CrystEngComm  (2017) –; doi:10.1039/C7CE01133D

data_7228856
_publ_section_title
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 Coordination polymers from a flexible alkyldiamine-derived ligand
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01133D
_journal_year                    2017
_chemical_formula_moiety         'C35 H36 N2 O8, 2(Cl), 3(H2 O)'
_chemical_formula_sum            'C35 H42 Cl2 N2 O11'
_chemical_formula_weight         737.60
_chemical_name_common            H6L1
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-15
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
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2017-06-16 deposited with the CCDC.
2017-08-04 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 95.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5650(17)
_cell_length_b                   10.777(2)
_cell_length_c                   37.736(8)
_cell_measurement_reflns_used    56815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.995
_cell_measurement_theta_min      1.084
_cell_volume                     3467.7(12)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  Synchrotron
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            56815
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.084
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XSCALE within XDS'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0355P)^2^+11.3639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6919
_reflns_number_total             8269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01133d2.cif
_cod_data_source_block           h6l1
_cod_database_code               7228856
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O11(H11A,H11B), O9(H9A,H9B), O10(H10A,H10B)
2.b Ternary CH refined with riding coordinates:
 N2(H2), N1(H1A)
2.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C28(H28A,H28B), C12(H12A,H12B), C4(H4A,H4B), C1(H1B,H1C),
 C3(H3A,H3B), C2(H2A,H2B)
2.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C34(H34), C22(H22), C30(H30), C23(H23), C26(H26), C10(H10), C6(H6),
 C7(H7A), C15(H15), C14(H14), C33(H33), C9(H9), C18(H18), C25(H25), C17(H17)
2.e Idealised tetrahedral OH refined as rotating group:
 O7(H7), O1(H1), O5(H5), O3(H3)
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_olex2_submission_special_instructions 'No special instructions were received'